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1375 results about "Protecting group" patented technology

A protecting group or protective group is introduced into a molecule by chemical modification of a functional group to obtain chemoselectivity in a subsequent chemical reaction. It plays an important role in multistep organic synthesis.

Method for preparing graphdiynyl material based on Sonogashira-Hagihara cross-coupling reaction

The invention discloses a method for preparing a graphdiynyl material based on a Sonogashira-Hagihara cross-coupling reaction, and belongs to the technical field of Sonogashira-Hagihara cross-coupling Reaction. According to the method, halogenated aromatic hydrocarbon and an alkynyl compound are used as raw materials, a palladium catalyst / copper catalyst is used as a catalytic system, and the graphdiynyl material is prepared by regulating the alkalinity and the polarity of a solvent. According to the present invention, the graphitized alkynyl material is obtained through the in-situ removal of the protection group on the acetylenic bond of the alkynyl compound and the Sonogashira-Hagihara cross coupling with the halogenated aromatic hydrocarbon, such that the method can select the variety of the halogenated aromatic hydrocarbon, the cost is low, the side reaction during the polymerization process is less, the variety of the graphitized alkynyl can be easily expanded, the development and the utilization of the high-quality graphitized alkynyl film can be easily achieved, and the method can be used for the preparation of the graphitized alkynyl material. The preparation cost of graphdiyne is reduced.
Owner:CHONGQING NORMAL UNIVERSITY

Gemigliptin oxalate as well as crystal form, preparation method and application thereof

The invention discloses a gemigliptin oxalate and a crystal form, a preparation method and application thereof, relates to the technical field of medicinal chemistry, and provides the crystal form of the gemigliptin oxalate, the crystal form is not reported in the prior art, and animal experiments show that compared with gemigliptin tartrate and gemigliptin hydrochloride, the crystal form of the gemigliptin oxalate has the advantages that the crystal form of the gemigliptin oxalate is more stable. The gemigliptin oxalate prepared by the invention has better pharmacokinetic performance, and lays a foundation for development and application of a new dosage form of gemigliptin; the invention further provides a simple and efficient gemigliptin salt forming process, compared with a method for removing an amino protecting group through acid treatment, the salt forming process provided by the invention does not need to add alkali to dissociate the amino group, impurity generation caused by strong acid or strong alkali is avoided, and the prepared gemigliptin oxalate is high in purity.
Owner:ANHUI HERYI CHEM

Preparation method of Omarlliptin

The invention relates to Omarlliptin, in particular to a novel method for preparing Istradafylline, and relates to a preparation method of Istradafylline, in particular to a preparation method of Istradafylline. The method comprises the following steps: carrying out coupling reaction on a compound Ia and TMS acetylene to obtain an intermediate Ib; carrying out bromination reaction on the intermediate Ic under the action of NBS (N-bromosuccinimide) to obtain an intermediate Id; carrying out substitution reaction on the intermediate Id and tert-butyl carbamate under the action of potassium tert-butoxide to obtain an intermediate Ie; reacting the intermediate Ie with paraformaldehyde to obtain an intermediate If; carrying out cycloaddition reaction on the intermediate If and the intermediate Ib to obtain a key intermediate Ig; carrying out asymmetric catalytic hydrogenation reduction on the intermediate Ig to obtain an intermediate Ih; and removing a protecting group from the intermediate Ih in a hydrochloric acid and ethyl acetate system to obtain a final product. The method is short in route, simple and convenient to operate, mild in condition, high in reaction yield, environment-friendly and easy for industrial production, and dangerous and highly toxic products are prevented from being used and hazardous chemicals are supervised. # imgabs0 #
Owner:STANDE STANDARD TECH RES (HUBEI) CO LTD

Solid-liquid combined synthesis method of semeglutide

The invention provides a solid-liquid combined synthesis method of semeglutide, which belongs to the technical field of semeglutide synthesis, and specifically comprises the following steps: segmenting a main chain of the semeglutide into three shorter polypeptide fragments, namely a fragment 4, a fragment 5 and a fragment 2 at sites 7-14, 15-22 and 23-37, and respectively synthesizing at the same time; performing solid-phase assembly on the fragment 4 and the fragment 5 to form 7-22 peptide fragments, namely a fragment 1, and after the fragment 1 is cut off from the resin, forming NHS ester at a C end; after the fragment 2 is assembled, selectively removing a protecting group A11oc on the Lys26, then connecting with a side chain for fatty acid treatment to form a fragment 3, and cutting off the fragment 3 from the resin; and connecting the NHS ester of the fragment 1 with the fragment 3 in a liquid phase reaction system. The crude semeglutide prepared by the synthetic method is relatively high in yield and purity. The refined semeglutide of which the purity is more than 99.3% and the content of single impurity is less than 0.1% can be obtained at high yield through a conventional purification means.
Owner:SICHUAN OPEN MEDICINE CO LTD

Solid-phase synthesis method of semeglutide

The invention provides a solid-phase synthesis method of semeglutide, and belongs to the technical field of synthesis of medical intermediates, and the method specifically comprises the following steps: segmenting a semeglutide main chain into three shorter polypeptide fragments, namely a fragment 4, a fragment 5 and a fragment 2, which are 7-14 sites, 15-22 sites and 23-37 sites; and respectively synthesizing and then assembling fragments to obtain a target product. The method specifically comprises the following steps: a) synthesizing a 7-14 peptide fragment and a 15-22 peptide fragment, and assembling the 7-14 peptide fragment and the 15-22 peptide fragment into a 7-22 peptide fragment, namely a fragment 1; b) synthesizing a 23-37 peptide fragment, selectively removing a protecting group A11oc on Lys26, and connecting with a side chain to form a fragment 3; c) connecting the peptide fragment 7-22 with the peptide fragment 23-37, and removing a protecting group to obtain a crude product; and d) separating and purifying to obtain a finished product. According to the invention, the purpose of high-purity, high-yield and low-cost synthesis of the semeglutide bulk drug can be achieved.
Owner:SICHUAN OPEN MEDICINE CO LTD

Method for preparing semeglutide by one-pot method

The invention discloses a one-pot preparation method of semeglutide, and relates to the field of polypeptide synthesis. The preparation method comprises the following specific steps: 1) taking Arg34GLP-1 (9-37) as a starting material, controlling the pH value of a reaction solution, enabling activated dipeptide Fmoc-His-Aib-OH to react with the starting material to obtain an acylation reaction solution, and directly carrying out next-step reaction without aftertreatment after the reaction is finished; 2) adjusting the pH value of the acylation reaction liquid I, adding a compound 2-tetrapeptide into the acylation reaction liquid I, reacting to obtain acylation reaction liquid II, and directly carrying out next-step reaction without post-treatment after the reaction is finished; (3) adding an alkaline reagent to remove the Fmoc protecting group, settling, centrifuging and drying to obtain a crude product of the semeglutide; 4) separating and purifying the crude product to obtain a refined semeglutide product; the first three steps are carried out in the same reactor. Compared with a conventional liquid-phase synthesis method, the preparation method disclosed by the invention is simpler and more convenient, short in construction period, low in output of waste liquid and waste water, greatly reduced in cost, higher in yield and suitable for large-scale production.
Owner:NANJING HANXIN PHARMA TECH CO LTD

Preparation method and intermediate of alasset hydrochloride

The invention provides a preparation method and intermediates of alasset hydrochloride, which comprises the following steps: reacting an initial raw material as shown in a formula 1, which is protected by bare phenolic hydroxyl groups or different protecting groups, with bis (pinacolato) diboron to obtain an intermediate as shown in a formula 2, carrying out coupling reaction on the intermediate and a compound as shown in a formula 3 to obtain a corresponding hydroxyl-protected intermediate as shown in a formula 4, and separating and purifying the intermediate to obtain the alasset hydrochloride. The preparation method comprises the following steps: carrying out catalyst pressurized hydrogenation, carrying out asymmetric chiral hydrogenation to obtain an intermediate as shown in a formula 5, carrying out substitution or reductive amination to obtain an intermediate as shown in a formula 6, carrying out nucleophilic substitution on the intermediate as shown in a formula 7 to obtain an intermediate as shown in a formula 8, and carrying out deprotection to obtain a target product as shown in a formula I. According to the invention, a chiral resolution link in the existing preparation technology is avoided, and a chiral group is introduced through asymmetric hydrogenation, so that the yield is greatly improved, the production cost is greatly reduced, the tedious and tedious synthesis steps in the original process are shortened, and the post-treatment is simpler and more controllable.
Owner:HANGZHOU NUOAO BIOMEDICAL TECH CO LTD

Adamantane modification-based antibacterial peptide simulant and application thereof

The invention discloses an antibacterial peptide simulant based on adamantane modification and application of the antibacterial peptide simulant. The preparation method comprises the following steps: performing amide condensation on Fmoc amino acid to obtain a compound of which the carboxyl terminal is modified by amantadine or Boc protected aliphatic amine, and then removing an Fmoc group by piperidine to obtain a series of amantadine modified crude products and Boc protected aliphatic amine modified intermediate compounds; the intermediate compound is subjected to amide condensation to obtain a compound of which the amino terminal is further modified by adamantanic acid, then other protecting groups are cracked by trifluoroacetic acid to obtain a series of adamantanic acid modified crude products, and the crude products are purified to obtain the adamantane modified peptidomimetic. The adamantane modified peptidomimetic is used for preparing drugs for treating infectious diseases caused by sensitive bacteria and drug-resistant bacteria, has efficient antibacterial activity and low toxicity, and is not influenced by a traditional drug-resistant mechanism.
Owner:LANZHOU UNIV

A method for synthesizing elastatin and its intermediates

The present invention provides a method for synthesizing alacastran, comprising reacting an amino compound of formula V with a chiral intermediate of formula VI, reducing the resulting product with a reducing agent capable of providing an ethyl group to produce a compound of formula VII, and then deprotecting the compound to obtain alacastran, as shown in the following reaction formula. The method for synthesizing alacastran of the present invention avoids the low yield caused by amide reduction and the risk of substrate racemization, has a high yield, low material cost, safe operation, and is suitable for industrial production.
Owner:AURISCO PHARM(TIANJIN) INC +1

Vilbeglycolone intermediate compound as well as preparation method and application thereof

The invention discloses a vibeglycolone intermediate, a preparation method thereof and application of the intermediate in preparation of vibeglycolone, and belongs to the technical field of medicinal chemistry. The structural general formula of the vibeglycolone intermediate compound II disclosed by the invention is as follows: # imgabs0 # R1 is a silicon-containing hydroxyl protecting group. The invention also develops a new synthesis route of vibeglycolone by adopting the key intermediate, and by introducing a hydroxyl protecting group at the front end of the reaction, the stability of the intermediate compound is increased, the generation of oxidation impurities in the cyclization and hydrogenation process is effectively reduced, the purification problem in the synthesis process is greatly improved, the cost is saved, and the yield is increased. The synthesis efficiency is also improved, the obtained target compound vibeglycolone has higher purity, and the newly developed synthesis route is more suitable for industrial large-scale production.
Owner:ZHEJIANG CHARIOTEER PHARMA

An imidazole derivative, its preparation method and application

The present invention discloses an imidazole derivative, a preparation method thereof, and an application, belonging to the field of organic chemistry. The preparation method of the imidazole derivative of the present invention includes: adding compound 2a and dimethyl sulfate into an organic solvent, heating and reacting to obtain compound 3a; wherein, compound 2a is prepared by adding compound 1a, TrtCl, and a base reagent into a solvent, controlling the temperature at 0-10 °C, mixing evenly and reacting. The present invention also further prepares 2-(1-methylimidazol-5-yl)ethylamine (4a) by using the imidazole derivative. The present invention selects dimethyl sulfate as a methylation reagent and cooperates with a specific protecting group design to achieve the efficient preparation of 2-(1-methylimidazol-5-yl)ethylamine, with a total yield of 82.4%.
Owner:JIANGXI LINGFU BIOTECHNOLOGY CO LTD

Pharmaceutical intermediate and synthesis method, and isoquinoline derivative and synthesis method therefor

The present invention belongs to the technical field of drug synthesis, relating to the synthesis of drugs for the prevention or treatment of diseases such as Alzheimer's disease and Parkinson's disease. Specifically, it relates to pharmaceutical intermediates and synthesis methods and isoquinoline derivatives and synthesis methods therefor. The pharmaceutical intermediate has a chemical structure shown in Formula II, wherein X is a halogen, and R is an amino protecting group. The synthesis of the pharmaceutical intermediate is simple, operates under mild conditions, and results in a high yield. Additionally, the pharmaceutical intermediate can be used to prepare isoquinoline derivatives.
Owner:BANGENTAI (SHANDONG) BIOSCIENCES GRP SHARE CO LTD

Synthesis process of vitamin C ethyl ether

The invention discloses a synthesis process of vitamin C ethyl ether, and belongs to the technical field of vitamin C derivative synthesis. The process comprises the following steps: taking L-ascorbic acid as a raw material, adding acetone, anhydrous cupric sulfate and acetyl chloride, and reacting for 1-2 hours at 38-40 DEG C under the protection of nitrogen to obtain a vitamin C protector; adding alkali, water, an alkylating reagent and absolute ethyl alcohol into the reaction product, reacting for 3 hours at 75-78 DEG C under the protection of nitrogen, and performing reduced pressure distillation to obtain a vitamin C protector etherate; and finally, hydrolyzing by using cationic resin, removing a protecting group, and recrystallizing by using ethyl acetate to obtain the vitamin C ethyl ether. Through the synergistic catalysis of anhydrous cupric sulfate and acetyl chloride, the reaction time is remarkably shortened, and the product purity and yield are improved. Through detection, the product purity is more than 99.5%, the total yield can reach more than 80%, and an efficient and economical method is provided for industrial production of vitamin C ethyl ether.
Owner:SHANGHAI JAKA BIOTECH CO LTD

Preparation method of < 18 > F-DOPA and F-18 labeled precursor of < 18 > F-DOPA

The invention relates to the technical field of biological medicines, in particular to a preparation method of 18F-DOPA and an F-18 labeled precursor of 18F-DOPA. The structural formula of the F-18 labeled phenolic precursor compound is as shown in a formula I: # imgabs0 #; wherein R1 and R2 are hydroxyl protecting groups; r3 is a leaving group; r4 and R5 are independently hydrogen or an amino protecting group; and R6 is a carboxyl protecting group. The invention provides a simple and efficient < 18 > F-DOPA preparation method, and particularly relates to preparation of < 18 > F-DOPA by constructing a key phenol precursor compound and performing a simple and efficient photocatalytic deoxidation fluorination reaction on aromatic hydrocarbon. The method has the advantages of few steps, high yield, simplicity and convenience in operation, good repeatability and good automatic production potential. The radioactive tracer agent 18F-DOPA synthesized by using the method has high specific activity, high chemical purity and high radioactive purity, and has an important value for clinical popularization of 18F-DOPA.
Owner:WEST CHINA HOSPITAL SICHUAN UNIV

Antibody-drug conjugate

The present invention provides a novel linker, a linker-payload, and an antibody-drug conjugate, as well as an antitumor drug. Specifically, the present invention provides an antibody-drug conjugate represented by the following general formula (I):         A-(B-L-D)a     (I) [wherein A is an antibody residue in which functional group(s) in antibody involved in binding to linker(s) is / are removed from an antibody which can target a tumor cell; B is a divalent group derived from said functional group in antibody; a is an integer of 1 to 10; D is an antitumor drug residue in which one hydrogen atom or one hydroxy group is removed from any position of an antitumor drug molecule or an analog thereof, or a derivative thereof; L is a linker which links B to D; and at least any one of D and L has one or more lactonyl group(s) as substituent(s) or protecting group(s) at any position(s)] or a pharmacologically acceptable salt thereof, or a hydrate thereof, and the like.
Owner:UBE CORPORATION

Synthetic method of glabridin

The invention discloses a synthetic method of glabridin with optical purity, which comprises the following steps: by taking (R)-3-acetoxyl-2-(2, 4-dimethoxyphenyl) propanol and 2-isopentenyl resorcinol as raw materials, carrying out Mitsunobu reaction to obtain a key intermediate compound I, then carrying out hydrolysis and iodination to obtain an intermediate compound II, and then carrying out cyclization to obtain the glabridin with optical purity. Reducing and removing a protecting group to obtain glabridin. By introducing the isopentene side chain, the reaction activity of an olefin functional group is reserved, a key site is provided for subsequent cyclization conversion, the precise spatial configuration of the product is ensured, and finally glabridin with optical purity is prepared. The method is short in route, low in cost, mild in reaction condition and suitable for industrial production.
Owner:TIANJIN TAIPU PHARMA SCI & TECH DEV

Acid-free thermal deprotection of trityl protected oligonucleotides

The present disclosure relates to methods of deprotecting a trityl-based protecting group from an amine group or a hydroxyl group of an oligonucleotide, such as an oligonucleotide modified with a 5'-amine group. The methods generally comprise heating the oligonucleotide in an acid-free aqueous solution at a temperature of at least 60°C, optionally with removal of an insoluble trityl-hydroxyl byproduct to further drive the deprotection reaction. The methods allow facile deprotection of trityl-based protecting groups with little or no depurination of the product oligonucleotide.
Owner:ELSIE BIOTECHNOLOGIES INC

Antibody-drug conjugate precursors and synthetic intermediates thereof

Provided are: a method for improving the stability of an antibody-drug conjugate in a living body; and a conjugate precursor for obtaining a stabilized antibody-drug conjugate. Specifically, the present invention provides an antibody-drug conjugate precursor represented by general formula (I): Z-L-D (I) or a salt thereof, a synthetic intermediate thereof or a salt thereof, and the like. [In the formula, Z is a reactive group capable of reacting with a functional group present in an antibody or a modified antibody, D is an antitumor drug residue obtained by removing one hydrogen atom or one hydroxyl group from any position of an antitumor drug molecule, an analog thereof, or a derivative thereof, L is a linker linking Z and D, and n is an integer from 1 to 2. And at least one of D and L has at least one lactone group as a substituent or protecting group at an arbitrary position].
Owner:UBE CORPORATION

Preparation method of nerofloxacin chiral piperidylamine intermediate

The invention relates to a method for preparing a nerofloxacin chiral piperidylamine intermediate, which comprises the following steps of: carrying out condensation reaction on 5-hydroxy nicotinic acid which is simple and easy to obtain and is used as a raw material and different alcohols, screening through a series of asymmetric catalytic hydrogenation conditions to obtain optimal reaction conditions, and under the conditions, carrying out reaction on various 3, 3 '-dihydroxy nicotinic acid and 3, 3'-dihydroxy nicotinic acid to obtain the nerofloxacin chiral piperidylamine intermediate. The 2, 5-disubstituted pyridine quaternary ammonium salt is reduced into a tetrahydropyridine product, and the C5 site enantioselectivity of the product is excellent. The preparation method comprises the following steps: selecting methyl (R)-1-benzyl-5-hydroxy-1, 4, 5, 6-tetrahydropyridine-3-carboxylic acid methyl ester as a substrate, completely hydrogenating by using platinum dioxide hydrogen, and then carrying out methyl ester reduction, dehydroxylation, Mitsunobu reaction and protecting group removal to obtain a key chiral intermediate for industrial synthesis of a quinolone antibacterial drug nemonofloxacin with high enantioselectivity and high yield.
Owner:SICHUAN UNIV

Bio-based MS resin and preparation method thereof

PendingCN120441744APolymer scienceCaffeic acid
The invention belongs to the technical field of polymer synthetic materials, and particularly relates to bio-based MS resin and a preparation method thereof. The bio-based MS resin is a free radical copolymer of a methyl methacrylate monomer and a styrene monomer; the methyl methacrylate monomers comprise bio-based methyl methacrylate, isobornyl methacrylate and 3-pinane methacrylate, and the methyl methacrylate monomers comprise methyl methacrylate, isobornyl methacrylate and 3-pinane methacrylate; the styrene monomers comprise styrene and caffeic acid derivatives; based on 100% of the mass of the bio-based MS resin, the methacrylate monomer accounts for 30%; the molar ratio of caffeic acid derivatives to styrene in the styrene monomers is 1: (1-9). The synthesized bio-based MS resin has the characteristics of greenness and reproducibility, compared with petroleum-based MS resin, the performance of the MS resin can be regulated and controlled by designing a protecting group of a bio-based caffeic acid derivative so as to expand the application range of the MS resin, a specific functional group can be introduced to prepare a functional, advanced and high-performance polymer material, and the MS resin has a good market prospect.
Owner:DALIAN UNIV OF TECH

Synthesis method of retaglutide and retaglutide

The invention relates to the technical field of polypeptide synthesis, in particular to a synthesis method of retaglutide and the retaglutide prepared by the method. Comprising the following steps: synthesizing retaglutide side chain peptide resin through an Fmoc / tBu solid phase method; removing a Lys17 main chain protecting group Dde or Alloc, and sequentially coupling main chain protected amino acids or protected amino acid fragments to obtain retaglutide peptide resin; cracking the peptide resin by adopting an acidic mixed solution to obtain crude peptide; and performing HPLC (High Performance Liquid Chromatography) purification, salt conversion, concentration and freeze-drying on the crude peptide to obtain refined retaglutide. According to the retaglutide synthesis method provided by the invention, the purity of the obtained retaglutide product is greater than 99.0%, and the purity of a single impurity is less than 0.10%. The synthesis method is simple to operate, high in crude peptide purity, easy to purify and prepare, low in comprehensive synthesis cost and very suitable for industrial production.
Owner:HANGZHOU SINODA PHARM TECH CO LTD

Methods of preparing phosphonamidate compounds

The present invention relates to methods of preparing phosphonamidate compounds of, for example, formulae (I) and (II), or solvates or salts thereof: (I) (I*) wherein: - is a triple bond; or - is a double bond; - is absent when is a triple bond; or V is H or (C1-C8)alkyl when is a double bond; X is R3-C when is a triple bond; or X is R4-R5-C when is a double bond; R1 is an optionally substituted aliphatic residue or an optionally substituted aromatic residue; R3 is selected from the group consisting of H, –Si(RSi)3 and (C1-C8)alkyl, wherein RSi is, each independently, (C1-C8)alkyl; R4 is H or (C1-C8)alkyl; R5 is H or (C1-C8)alkyl; R6 is H or (C1-C8)alkyl; A is a spacer; and PG is a protecting group. The present invention also relates to phosphonamidate compounds of, for example, formulae (I) and (I*) or solvates or salts thereof.
Owner:TUBULIS GMBH

Coumarin tyramine glycoside compound and application thereof in preparation of PTP1B (protein tyrosine phosphatase 1B) inhibitor and antidiabetic drug

The invention discloses a coumarin tyramine glycoside compound and application thereof in preparation of PTP1B (protein tyrosine phosphatase 1B) inhibitors and antidiabetic drugs. The structural formula of the compound is # imgabs0 #, in the formula, R represents fat (aromatic) acyl or monosaccharide substituent, and R'represents hydrogen atom or acetyl; 4-methoxycoumarin 4 '-acetyl-O-L-rhamnose is used as an initial raw material, fat (aromatic) acyl or monosaccharide substituent groups are introduced into hydroxyl at the second position and hydroxyl at the third position of L-rhamnose at the same time, and then protecting groups of glycosyl are removed, so that the L-rhamnose is prepared. Pharmacological activity tests show that the compounds have good inhibitory activity on protein tyrosine phosphatase 1B, which indicates that the coumarin tyramine glycoside compounds can be researched and utilized as novel PTP1B inhibitors and antidiabetic drugs.
Owner:NORTHWEST UNIV

Chemical synthesis method of insulin analogue

The invention discloses a synthesis method of an insulin analogue, which comprises the following steps of: firstly, obtaining A-chain peptide resin by using a solid-phase synthesis method, constructing a disulfide bond between A6 and A11 on a solid phase, and cracking the A-chain peptide resin by using a cracking solution containing a sulfydryl activator to obtain a peptide chain with an activated sulfydryl group and a protected sulfydryl group; then a solid-phase synthesis method is used for obtaining B-chain peptide resin, Lys side chain protecting groups are removed on a solid phase in a fixed-point mode, side chain fatty acid modification is completed, and a peptide chain with an exposed sulfydryl group and a protected sulfydryl group is obtained after cracking is conducted through a cracking solution; and mixing the products in a solution according to a certain proportion to form a first pair of intermolecular disulfide bonds, and constructing and purifying the last pair of disulfide bonds to obtain the insulin analogue. The method disclosed by the invention has the advantages of convenience in synthesis, low cost, simple process and the like, can be used for research on amino acid mutation of insulin compounds, and has important practical significance on development of insulin drugs.
Owner:SHENZHEN TURIER BIOTECH CO LTD

Reagents and processes for preparing oligonucleotides

The present disclosure describes novel reagents and processes for preparing oligonucleotides, which have two or more nucleotides. In one embodiment, the reagent is represented by Formula I. wherein: W is O or NH; R1 is -H or a solid support; R2 is a silyl hydroxyl protecting group or an alloc protecting group, R3 is a nucleoside or a group represented by (II) wherein (III) represents the point of attachment for R3.
Owner:BIOGEN MA INC

Preparation method of alplsutentan and alplsutentan intermediate

The invention discloses a preparation method of alplsutentan and an alplsutentan intermediate, alplsutentan is obtained by taking a compound SM1 as a raw material through a one-step method or a multi-step method, and the multi-step method comprises the following steps: reacting the compound SM1 with a compound SM2 to obtain an intermediate I; reacting the intermediate I with 2-[(5-bromo-2-pyrimidinyl) oxy] ethanol to obtain an intermediate II, or reacting the intermediate I with ethylene glycol to obtain an intermediate I-b, and then reacting with 5-bromo-2-chloropyrimidine or 5-fluoro-2-chloropyrimidine to obtain the intermediate II; and finally, removing a protecting group from the intermediate II to obtain alpoxivan. The one-step method comprises the following steps: when X in a compound SM1 is a fluorine atom, the compound SM1 is 5-(4-bromophenyl)-4, 6-difluoropyrimidine, and the compound SM1 reacts with sulfonamide and 2-[(5-bromo-2-pyrimidinyl) oxy] ethanol to directly obtain alpoxivan. The synthesis route is short, and the reaction conditions are mild.
Owner:NANJING DOYLE PHARM RES INST CO LTD

Method for preparing zavegepant intermediate and derivative thereof

The present invention relates to the field of drug synthesis, and specifically relates to a method for preparing a Zavegepant intermediate and a derivative thereof. Specifically, the method comprises reacting a compound of formula II with a compound of formula III to obtain a compound of formula I, reacting the compound of formula I with isoamyl nitrite to obtain compound V, and removing a protecting group from the compound of formula V to obtain a compound of formula VI or a salt thereof. On the basis of the preparation method provided by the present invention, the raw materials are readily available, the production cost is relatively low, there are fewer synthesis steps, and the operation is simpler and more convenient.
Owner:SHANGHAI SYNCORES TECH INC +1

Preparation method of polypeptide with anti-inflammatory effect

The invention discloses a preparation method of polypeptide with an anti-inflammatory effect. The preparation method comprises the following steps: S1, swelling resin; s2, removing Fmoc protecting groups of the resin; s3, washing the resin, and draining the cleaned resin to ensure that the resin reaches the cleanliness required by the next-step reaction; s4, amino acid coupling; s5, removing an Fmoc protecting group in the amino acid; s6, polypeptide cutting: preparing a cutting reagent, after the last amino acid is synthesized and the Fmoc group is removed, cleaning the resin, adding the cutting reagent, putting a synthesis tube into a shaking table, oscillating, cutting, collecting a cutting liquid into a centrifugal tube, and drying by blowing; s7, polypeptide purification; and S8, polypeptide freeze-drying: performing freeze-drying treatment on the purified polypeptide solution through a low-temperature freeze-drying machine to finally obtain solid powder of the target polypeptide. The anti-inflammatory effect can be improved, adverse reactions are reduced, toxic and side effects on the body in the anti-inflammatory process are reduced or eliminated, and the varieties of anti-inflammatory polypeptides are enriched.
Owner:ZHEJIANG LANSHU COSMETICS CO LTD

A pag key type photosensitive photoresist resin and a preparation method thereof

The application discloses a PAG bonding type photosensitive photoresist resin and a preparation method and application thereof. The photoresist resin is as follows: formula. The PAG bonding type resin is prepared through the following reaction process: 1) performing a RAFT polymerization reaction on p-acetoxystyrene, p-styrene sulfonamide trifluoromethyl potassium salt and a RAFT chain transfer agent under the action of an initiator to obtain an intermediate I, 2) performing a hydrolysis reaction on the intermediate I to obtain an intermediate II, 3) performing a protection group introduction reaction on the intermediate II and di-tert-butyl dicarbonate to obtain an intermediate III; and 4) performing an ion exchange reaction on the intermediate III and triphenylsulfonium bromide. The application realizes the bonding of the PAG into the resin skeleton, and improves the problems of poor compatibility between the PAG and the resin, phase separation, uneven distribution of the PAG and the like. Therefore, the photoresist prepared from the resin has the photo-generated acid bound by the polymer main chain and limited diffusion, the resolution is improved, and the photoetching effect is excellent.
Owner:HANGZHOU XIANYAN TECH CO LTD +1

Four acinetobacter baumannii cell wall oligosaccharide fragments as well as synthesis method and application thereof

The invention belongs to the field of chemical synthesis, and particularly relates to four acinetobacter baumannii cell wall oligosaccharide fragments as well as a synthesis method and application thereof. Four acinetobacter baumannii core oligosaccharide fragments are synthesized by adopting a divergent synthesis strategy, compounds 1-3 take orthogonally protected alpha-(2-> 5)-Kdo-Kdo disaccharide as key precursors, protecting groups at different sites are selectively removed, glycosyl is introduced through a stereoselective glycosylation reaction, and thus a target molecular skeleton is constructed. The method disclosed by the invention and the four finally prepared acinetobacter baumannii core oligosaccharide fragments have huge industrial application potential.
Owner:SICHUAN UNIV