18 results about "Annulation" patented technology

The application discloses application of a divinyl tetrazine in cyclization of a linear polypeptide, and a structure formula of the divinyl tetrazine is; the linear polypeptide has at least two free mercapto groups, and the vinyl groups of the divinyl tetrazine are subjected to Michael addition reaction with corresponding mercapto groups to form a ring. The application provides a new use of the divinyl tetrazine, the divinyl tetrazine can be subjected to high-efficiency Michael addition reaction with two natural cysteine mercapto groups on the linear polypeptide through the vinyl groups, so that double-mercapto peg cyclization of the linear polypeptide is realized, and the purpose of limiting the conformation of the linear polypeptide and improving the stability of the linear polypeptide is achieved. Moreover, the divinyl tetrazine can be subjected to a reverse electron demand Diels-Alder reaction with trans-cyclooctene (TCO) after the two vinyl groups are subjected to reaction with mercapto groups, so that functional polypeptides can be modularly constructed by coupling with functional molecules modified with TCO, and related applications are realized.

The application relates to the field of polypeptide medicine preparation, and particularly discloses a preparation method of bumenol peptide, which adopts a solid-liquid combination mode, liquid-phase synthesis of a tripeptide fragment Fmoc-Lys(Ac-Nle-Asp)-OMe, subsequent solid-phase synthesis of a cyclic heptapeptide methyl ester, cleavage, cyclization, deprotection and hydrolysis to obtain crude bumenol peptide. The cyclization site is alpha-COOH of Trp and alpha-NH2 of Lys, the reaction yield is high, and the cyclization problem between Lys and Asp in most current patents is solved. The process operation is simple, the deprotection reagent is conducive to environmental protection requirements. The crude product is easy to purify, the finished product has high yield and purity, and is suitable for industrial large-scale production.

The patent application discloses a kind of polyquinoline acridinedione macrocyclic derivatives and its preparation method and application.The application is by methylene bridging, multiple single-molecule fragments of quinoline acridinedione is gathered into macrocycle, the difference between the electron-withdrawing and electron-donating properties of carbonyl and nitrogen atom is synthesized into a variety of quinoline acridinedione macrocyclic derivatives containing the relative distribution structure of carbonyl and nitrogen atom, the interaction of carbonyl and nitrogen atom heterocycle is conducive to realize high color purity molecular luminescence.Because the free rotation of benzene ring and intramolecular vibration caused by single fragment molecule itself is not fixed, energy is attenuated in the form of non-radiative transition, and the benzene ring after being polymerized into ring can efficiently emit light due to the limited rotation, and improve the color purity of luminescence.

The invention relates to a preparation method of a baloxvir intermediate, and belongs to the technical field of medicine synthesis. The preparation method comprises the following steps: reacting a compound 02 with 2-fluorobenzaldehyde in the presence of an alkaline reagent, and carrying out post-treatment to obtain a compound 03. And carrying out cyclization reaction on the compound 03 in the presence of acid to obtain a compound 04. The preparation method provided by the invention is short in reaction time, mild in reaction, easy in reagent obtaining, safe to operate, high in product yield, high in product purity, capable of reducing the cost and beneficial to industrial implementation.

The application provides a preparation method of an electrocatalytic SCF-substituted dihydrofuran compound, and belongs to the technical field of compound preparation. The application uses diazonium and ethylene compounds as substrates, uses an SCF source as a sulfur-containing and fluorine-containing fragment donor, realizes a one-pot cascade reaction of ring formation through electrolysis, and thus constructs the SCF-substituted dihydrofuran compound. The raw material of the application has a wide source, uses electric current as a reaction driving force, avoids or reduces the use of additional photosensitizers and chemical oxidation-reduction reagents, and has the one-pot cascade characteristics of ring C-N bond breaking, C-O bond construction, trifluoromethylation and ring formation and the like, so that the step economy can be improved.

The application discloses a kind of modified carboxylate macrocyclic molecules and preparation method and application thereof, it is related to organic material and electroluminescent device technical field;Macrocyclic molecules include molecular structure formula I and molecular structure formula II, and the macrocycle of it respectively contains 8 and 10 1,4-para phenylene, R in structure can be selected variously;Its synthesis method includes the steps of gradually connecting carboxylate monomer, using template to guide ring formation, intramolecular ring closure reaction and palladium catalysis reaction;Device based on this molecule has electronic device, hole device and OLED device, all contain functional film layer, and preparation method is various;The molecule and device of the application have outstanding photoelectric performance, can reduce intermolecular force, reduce π-π stacking, improve solubility, reduce device start-up voltage, control luminescent color;Through application in different devices, provide a new solution for related field, with wide application prospect.

The invention relates to a piperidine functionalized ring-containing polyfluorene ether ketone anion exchange membrane and a preparation method thereof. The preparation method comprises the following steps: reacting tetramethyl bisphenol fluorene with excessive 4, 4 '-difluorobenzophenone to generate an ABA type compound containing four methyl groups, performing cyclization reaction on the ABA type compound and tetramethyl dimethoxy bisphenol fluorene in a dilute solution to obtain a dimethoxy group-containing cyclic compound, reacting the dimethoxy group-containing cyclic compound with boron tribromide to prepare a cyclic monomer containing two phenolic hydroxyl groups, and reacting the cyclic monomer with 4, 4'-difluorobenzophenone to obtain a dimethoxy group-containing cyclic monomer. The preparation method comprises the following steps: carrying out polycondensation on 4, 4 '-difluorobenzophenone and bisphenol fluorene at a high temperature to prepare a ring-containing polyfluorene ether ketone compound, brominating methyl in the ring-containing polyfluorene ether ketone compound by utilizing bromination reaction, reacting with N-methylpiperidine to prepare a piperidine functionalized ring-containing polyfluorene ether ketone compound, and carrying out solution casting to obtain the anion exchange membrane. The obtained anion exchange membrane has the advantages of high ion conductivity, low vanadium ion permeability, high mechanical strength and the like.

The application discloses a preparation method of 4-[2-[(2-methoxyethoxy)methoxy]ethyl]morpholine, which comprises two steps of reactions: in the first step, triethanolamine is used as a starting material, and intramolecular dehydration and ring formation reaction occur under the action of a catalyst iron trichloride, so that an intermediate N-hydroxyethyl morpholine is obtained after rectification; in the second step, nucleophilic substitution reaction occurs between the intermediate and 2-methoxyethoxymethyl chloride in an organic solvent under the action of an acid binding agent, so that 4-[2-[(2-methoxyethoxy)methoxy]ethyl]morpholine crude product is obtained after extraction, water removal and solvent rotary evaporation, and the crude product is purified to obtain 4-[2-[(2-methoxyethoxy)methoxy]ethyl]morpholine product; the use amount of the catalyst iron trichloride in the first step is 2% to 4% of the mass of the triethanolamine; and the mass ratio of the intermediate to the 2-methoxyethoxymethyl chloride is 1:1.2 to 1.4; the product prepared by the method has a purity meeting the demand of electronic chemicals, provides a raw material basis for subsequent research in the photoresist field, and has high industrial popularization value.

The application discloses a preparation method of an intermediate of Axitinib and an intermediate of Axitinib as shown in formula VI. The application provides a preparation method of a compound as shown in formula VII, which comprises the following steps: performing ring formation reaction on a compound of formula VI in the presence of a base and a solvent to obtain the compound of formula VII. The Axitinib synthesis route provided by the application has the advantages of less steps, low cost, high purity of a synthesis product and no introduction of toxic substances.

The application belongs to the technical field of organic synthesis, and particularly relates to an asymmetric total synthesis method of catharanthine. Commercially available oxazolidinone 1 is used as a starting material, and is condensed with bromoacrylic acid to obtain compound 2. Then, asymmetric DA reaction of compound 2 and compound 3 occurs under the catalysis of scandium triflate to obtain compound 4. Compound 4 is hydrolyzed into a carboxylic acid under the condition of lithium hydroxide and hydrogen peroxide, and is treated by trimethylsilane diazomethane to obtain compound 6. Compound 6 is selectively reacted with sodium methoxide, and after the protective group is removed by treatment of iodo-trimethylsilane, compound 6 is condensed with an acid to obtain compound 9. Compound 9 is subjected to radical annulation under the catalysis of a photocatalyst Ir(ppy)3 to obtain compound 10. Finally, selective reduction of the amide obtains natural product (+) - catharanthine. The asymmetric total synthesis route of the application has a total step of 8 or 9, and a total yield of 17.8% - 23.5%, which is shorter than that of the prior art, and the total yield is significantly improved.

The invention discloses a preparation method of an optical pure amino acid herbicide. The preparation method comprises a preparation method of a refined glufosinate-ammonium intermediate. The method comprises the following steps: carrying out cyclization reaction on a compound as shown in a formula (III) and a compound as shown in a formula (IV) in the presence of a solvent and organic alkali to obtain a compound as shown in a formula (V), and then carrying out intramolecular Arbuzov rearrangement reaction under the action of a halogenation catalyst to obtain the refined glufosinate-ammonium intermediate. The preparation method is simple in process, the synthesis route is reduced, complex and tedious separation and purification processes are avoided in the synthesis steps, particularly, waste salt, waste acid and toxic waste gas are not generated in the aspect of three-waste control, and the product quality is high. In addition, the reaction conditions are mild, the operation is simple, the continuity among the working sections is strong, the raw material cost and the industrial investment are effectively reduced, and the trend of green chemical industry is met.

The application discloses a preparation method of a heterocyclic alkyl compound, an intermediate thereof and application of the intermediate. The application provides a preparation method of a compound shown in a formula IN-06, which comprises the following steps: performing ring formation reaction and deprotection reaction on a compound shown in a formula IN-05 in an organic solvent in the presence of an acid-binding agent to obtain the compound shown in the formula IN-06, and the acid-binding agent is NaOH, NaH or potassium carbonate; wherein R is halogen. The preparation method has one or more advantages of higher chiral purity and being beneficial to industrial production.

The invention discloses an internal electron donor regulator, a solid catalyst component and a preparation method and application thereof. The internal electron donor regulator comprises at least one of compounds with a structure as shown in the following formula (I), r1 and R1'are the same or different, and are respectively and independently one of hydrogen, halogen, hydroxyl, C1-C30 straight-chain alkyl containing or not containing a substituent group, C3-C30 branched-chain alkyl containing or not containing a substituent group, C2-C30 alkenyl containing or not containing a substituent group, C2-C30 ester group containing or not containing a substituent group, C6-C30 aryl containing or not containing a substituent group, and C3-C30 cycloalkyl or heterocyclic radical containing or not containing a substituent group; r1 and R1'can form a ring at will; r < 2 >, R < 3 >, R < 4 >, R < 5 >, R < 2 '>, R < 3' >, R < 4 '> and R < 5' > are the same or different and are respectively and independently one of hydrogen, halogen, hydroxyl, nitryl, amino, C1-C30 linear alkyl containing or not containing substituent groups, C3-C30 branched alkyl containing or not containing substituent groups, C2-C30 alkenyl containing or not containing substituent groups, C6-C30 aryl containing or not containing substituent groups, and C3-C30 cycloalkyl or heterocyclic radical containing or not containing substituent groups; any two of R2, R3, R4, R5, R2 ', R3', R4 'and R5' can form a ring at will; a is selected from one of alkylene, arylene, heteroarylene, alkyl arylene and aryl alkylene which contain or do not contain substituent groups. When the compound with the structure as shown in the formula (I) and the existing internal electron donor compound are used together, the performance of the internal electron donor can be effectively improved, and the obtained catalyst has higher catalytic activity and orientation capability, and can adjust the molecular weight distribution of a polymer to obtain a polyolefin product with moderate molecular weight distribution.

The application provides a synthesis method and application of a selenocysteine-mediated cyclic peptide. A substrate polypeptide is synthesized by a solid-phase polypeptide synthesis method, the C terminal of the substrate polypeptide exists in a hydrazine form, and the N terminal of the substrate polypeptide is selenocysteine. A cyclization method is used to add ascorbate, high-concentration tris(2-chloroethyl) phosphate (TCEP) and acetylacetone to the substrate polypeptide, and the reaction is carried out at room temperature by oscillation to obtain a corresponding target cyclic peptide. The application helps to expand the synthesis method of the cyclic peptide with a ring structure at the head and tail, and realizes efficient synthesis of the cyclic peptide.

This invention relates to the field of gas purification and discloses a desulfurization absorbent, which, by weight, contains 1-20 parts by weight of an organic guanidine base and 10-70 parts by weight of an alkanolamine. The organic guanidine base has the structure shown in Formula I: Among them, R 1 R 2 R 3 R 4 R 5 Each is independently selected from hydrogen, substituted or unsubstituted alkyl, substituted or unsubstituted benzyl, or substituted or unsubstituted aromatic alkyl; or, R 5 With R 1 Or R 4 Ring formation, and / or R 2 With R 3 Cyclic formation. This desulfurization absorbent contains a specific amount of organic guanidine and a specific amount of alcoholamine, which can form a synergistic effect to improve the desulfurization efficiency of the desulfurization absorbent. In addition, the organic guanidine has a specific structure, which can effectively remove multiple harmful gases from sulfur-containing gases and selectively remove carbon dioxide, thereby improving the selectivity and stability of the desulfurization absorbent.

The invention relates to a preparation method of an intermediate for preparing 4-oxa-7-azaspiro [2.5] octane-6-ketone and an intermediate product of the intermediate, and belongs to the field of pharmaceutical chemical synthesis. Hydrochloride of glycine ester is used as a starting material, an intermediate product 2-(1-(aminomethyl) cyclopropoxy) acetate (VI) is obtained through a protective group introduction reaction, cyclization, condensation and protective group removal, the structural formula of the intermediate product is shown in the specification, and R2 is selected from-CH3,-CH2-CH3,-CH (CH3) 2 and-C (CH3) 3. The intermediate product is subjected to intramolecular cyclization to prepare 4-oxa-7-azaspiro [2.5] octane-6-ketone, and the 4-oxa-7-azaspiro [2.5] octane-6-ketone is used as an initial raw material for synthesizing anti-influenza virus drugs and analogues thereof.

This invention provides novel sulfate esters or salts thereof having two or more carbonyl groups, and surfactants. A compound, characterized by having the formula: R 1 -C(=O)-R 2 -C(=O)-R 3 -OSO3X represents this. (In the formula, R) 1 It is a straight-chain or branched alkyl group with 1 or more carbon atoms, or a cyclic alkyl group with 3 or more carbon atoms, wherein the hydrogen atoms bonded to the carbon atoms are not substituted or are substituted by hydroxyl groups or monovalent organic groups containing ester bonds. If it has 2 or more carbon atoms, it may contain a carbonyl group. If it has 3 or more carbon atoms, it may contain monovalent or divalent heterocycles, or it may be rolled into a ring. R 2 and R 3 Independently a single bond or a divalent linker. R 1 R 2 and R 3 The total number of carbon atoms is 6 or more. X is H, a metal atom, or NR. 4 4. Imidazolium with or without substituents, pyridinium with or without substituents, or phosphonium with or without substituents, R 4 It can be an H or an organic group, and can be the same or different. R 1 R 2 and R 3 (In this context, any two elements can bond together to form a ring.)

The invention discloses a high-purity alaraniset intermediate compound and a preparation method thereof, and belongs to the technical field of drug synthesis, the structural formula of the intermediate compound is 1, 6-benzyloxy-1-hydroxy-2-bromo-3, 4-dihydronaphthalene, the preparation method comprises the following steps: 1, reacting 6-benzyloxy-1-hydroxy-2-bromo-3, 4-dihydronaphthalene with m-methoxybenzoyl chloride to form ester, and then reacting the ester with m-methoxybenzoyl chloride to form ester; carrying out intramolecular Friedel-Crafts alkylation reaction under the catalysis of Lewis acid to form a ring; step 2, performing alkaline high-temperature hydrolysis on the product in the step 1 to remove hydroxyl into double bonds and carboxylic acid; and step 3, enabling the product obtained in the step 2 to react with DPPA, and carrying out rearrangement reaction to obtain the 7-benzyloxy-3-(4-methoxy-2-Boc aminobenzene)-1. When 1, 6-benzyloxy-1-hydroxy-2-bromine-3, 4-dihydronaphthalene provided by the invention is used as a raw material to synthesize an ilastrant intermediate, expensive noble metal catalysis is avoided, the total yield can reach 35% or above, the purity can reach 99.6%, and the product can be stably prepared through a simple process and is suitable for industrial production.