296 results about "Di-tert-butyl dicarbonate" patented technology

The invention relates to a synthesis method of amino-protecting glycine dipeptidase derivant. The amino-protecting glycine dipeptidase derivant is N-9-Fmoc glycine dipeptidase, N-Boc glycine dipeptidase and N-acetyl glycine dipeptidase. The invention has the technology that glycine dipeptidase is dissolved in 1-20% of inorganic aqueous alkali, and the organic solution of Fmoc-OSu or Boc2O or Ac2Ois dropwise added; reaction is finished within 1-12 hours, the yield of the product Fmoc-Gly-Gly-OH, Boc-Gly-Gly-OH and Ac-Gly-Gly-OH is between 80-95%, and the content of the product is above 99%. The invention has simple technology, easy industrialization and low cost. The product of the invention is the important raw material for synthesizing polypeptide compound.

The invention discloses a method for preparing chiral N-tert-butyloxycarboryl-3-hydroxypiperidine. The method comprises the following steps: a) enabling racemic 3-hydroxypiperidine and di-tert-butyl dicarbonate ester to react to generate racemic N-tert-butyloxycarboryl-3-hydroxypiperidine; b) oxidizing the racemic N-tert-butyloxycarboryl-3-hydroxypiperidine into racemic N-tert-butyloxycarboryl-3-piperidone under the action of an oxidizing agent; c) reducing the racemic N-tert-butyloxycarboryl-3-piperidone by using a ketoreductase into the chiral N-tert-butyloxycarboryl-3-hydroxypiperidine. Compared with the prior art, the method provided by the invention can be used to prepare the chiral N-tert-butyloxycarboryl-3-hydroxypiperidine with the optical purity of 99% by using the racemic 3-hydroxypiperidine as a raw material, in addition, the material is cheap and easy to get, the reaction condition is mild, the operation is simple and feasible, the production cost is greatly lowered, and great industrial application value is achieved.

The invention discloses a synthesis method for GHK tripeptide. A conventional liquid-phase synthesis method is adopted. The method comprises the following steps of protecting lysine by using p-nitrophenyl acetate, protecting dipeptide obtained by enabling Boc-Gly-OH to react with histidine by using di-tert-butyl dicarbonate, and enabling the protected dipeptide to react with the protected lysine to obtain the GHK tripeptide. According to the method, the p-nitrophenyl acetate is used for protecting the lysine, and can selectively acylate amino groups farther away from carboxylic acid functional groups, and compared with a conventional protecting method, the p-nitrophenyl acetate protecting method has the advantages that the operating steps are simple, and the production cost is lowered; the di-tert-butyl dicarbonate is used for protecting the dipepetide, so that the generation of other byproducts is reduced, the lipophicity of a chemical compound is improved, the separation and purification of a product are facilitated, the yield of the product is improved, and meanwhile, the generation of a recemization product can also be reduced.

Synthesis of antineoplastic Melphalan is carried out by esterification reacting, amino-protection reacting, hydrogenation reducing, hydroxyethylation reacting, chlorination reacting, de-protection reacting, taking chlorinating agent, absolute alcohol protecting carboxyl and pyrocarbonic di-tert-butyl protecting amino, hydrolyzing by hydrochloric acid to obtain final product. It's cheap, efficient and non-toxic, has gentle reactive condition and can be used for industrial production. It's cheap, convenient, efficient and non-toxic and can be used for industrial production.

A process for production of cyclopropyl-fused pyrrolidine-based inhibitors of dipeptidyl peptidase IV is provided which employs a BOC-protected amine of the structure

prepared by subjecting an acid of the structure

to reduce amination by treating the acid with ammonium formate, nicotinamide adenine dinucleotide, dithiothreitol and partially purified phenylalanine dehydrogenase/formate dehydrogenase enzyme concentrate (PDH/FDH) and without isolating treating the resulting amine of the structure 2

with di-tert-butyl dicarbonate to form the BOC-protected amine.

The invention discloses a preparation method of a silodosin intermediate. The preparation method comprises the following steps that in an organic solvent, under the action of lewis acid, friedel-crafts acylation reaction occurs between a compound 2 and a compound 3, so as to obtain a compound 4, wherein the lewis acid is one of or more of zinc trifluoromethanesulfonate, bismuth trifluoromethanesulfonate, scandium trifluoromethanesulfonate and aluminum trichloride; under the action of organic acid or boron trifluoride ether complex, the compound 4 reacts with triethyl silicane, so as to obtain a compound 5; the compound 5 reacts with sodium azide, so as to obtain a compound 6; under the action of catalysts, the compound 6 reacts with di-tert-butyl dicarbonate ester and hydrogen, so as to obtain a compound 7; under an acidic condition, the deamination protective reaction of the compound 7 occurs, so as to obtain a compound 8; the compound 8 reacts with L-tartaric acid, so as to obtain a compound 1, namely the silodosin intermediate. The preparation method of the silodosin intermediate has the advantages of simplicity, economy and mild reaction conditions, and chiral resolution is not needed.

The invention relates to an amlodipine besylate compound and a novel preparation method thereof, wherein the method comprises the following steps that: a moderate amino-protecting reagent of di-tert-butyl dicarbonate is adopted so that the introduction of a Boc protecting group is realized, through the reaction of intermediums of 3-amino-crotonic acid methyl ester and 2-chlorobenzaldehyde, the obtained amlodipine besylate compound is directly carried out BOC protecting group removal reaction with benzene sulfonic acid, and the final product is obtained. Consequently, the invention is dispensed with the special deprotection step, simplifies the reaction steps, is more suitable for industrialized production and has high total reaction yield.

The invention relates to a preparation method of a liquid carbon dioxide thickening agent for unconventional oil and gas reservoir development, and can solve the problem of damage to an oil and gas reservoir in a conventional mining mode. The preparation method has the technical scheme that methylbenzene and water are added into a bottle; then, serinol is added; terbutyloxycarbonyl anhydride is dropwise added at 0 DEG C; reaction is performed for 4h at 25 DEG C; distillation is performed to obtain an intermediate product (1); then, perfluoro caprylic acid is added into another bottle; thionyl chloride and N,N-dimethyl formamide are added at 75 DEG C; reaction is performed for 2h; distillation is performed to obtain an intermediate product (2); next, the intermediate product (1) is added into another bottle; the temperature is raised to 75 DEG C; the intermediate product (2) is dropwise added; reaction is performed for 12h at 75 DEG C to obtain an intermediate product (3); finally, dichloromethane and trifluoroacetic acid are added into the bottle; then, the intermediate product (3) is added; reaction is performed for 2h at 25 DEG C; after extraction and vacuum drying, hexamethylene diisocyanate is added to perform reaction for 2 minutes; a final product is obtained. The thickening agent can increase the carbon dioxide viscosity, and can be used for fracturing reformation.

The invention relates to a tyrosine phthalocyanine derivative which has a structural general formula as the right, in the formula, M is equal to Zn or Al, R is equal to H, Na or CH2CH3. The preparation method for the tyrosine phthalocyanine derivative is: (1) an intermediate II is obtained through the reaction of tyrosine and 4-nitrophthalic nitrile with protected amino group; (2) an intermediate III can be obtained by detracting Boc in the solution of dichloromethane and trifluoroacetic acid; (3) the tyrosine phthalocyanine derivative I can be obtained by cyclizing of the dinitriles intermediate that comprises the tyrosine; wherein, the Boc is di-tert-butyl dicarbonate, a DMF is N, N-dimethylformamide, and a DBU is 1,8-diazacyclo(5,4,0)hendecene-7. The invention also comprises the application of the tyrosine phthalocyanine photosensitizers in preparing photodynamic medicines.

The invention discloses a filgotinib synthetic method and belongs to the technical field of chemical synthesis of medicines. 6-chloro-2-aminopyridine and di-tert-butyl dicarbonate ester are subjected to condensation reaction to obtain 6-chloro-2-tert-butyloxycarbonyl aminopyridine; hydrolysis reaction is performed; the obtained 6-chloro-2-tert-butyloxycarbonyl aminopyridine and trifluorinated methyl sulfonic anhydride are subjected to trifluoromethanesulfonic acid esterification reaction; the obtained 2-tert-butyloxycarbonylamino-6-pyridyltrifluoromethanesulfonate and [(1,1-dioxo-4-thiomorpholinyl)methyl]benzo-4-boronic acid pinacol ester are subjected to condensation reaction to obtain a tert-butyl ester derivative; the tert-butyl ester derivative is treated by trifluoroacetic acid and subjected to de-protection; the obtained intermediate and ethoxycarbonyl isothiocyanate are subjected to isothiocyanate reaction; the obtained intermediate and hydroxylamine hydrochloride are subjected to ring closing reaction; the obtained intermediate and cyclopropane carbonyl chloride are subjected to amidation reaction to obtain the finished product. Operation is simplified; reagents are available; the concept of environment friendliness and environment protection is embodied.

The invention relates to a method for preparing macroporous adsorbent resin special for separating valine, and belongs to the technical field of chemical and biological product processing. In the method, the types and proportions of an aqueous phase matter, cross-linking agents, polar monomers and pore-foaming agents are controlled in the process of synthesizing the resin, so that the resin can be bonded with di-tert-butyl dicarbonate effectively, and the synthesized macroporous adsorbent resin can separate the valine, alanine and leucine; and simultaneously, the macroporous adsorbent resin adopts pure water as a mobile phase, so that the pollution of a separation process on environment can be lightened effectively. The resin synthesized by the method can be effectively used for separating valine fermentation liquor and removing impurities with similar properties such as the alanine and the leucine in the valine fermentation liquor, and overcomes the defects of low purity, low efficiency, severe pollution and the like which exist in the conventional process for separating and purifying the valine, so that the purity of products reaches over 99 percent, reaches medicinal standards, and has high recovery rate and production strength.

The invention discloses a production method of fasudil hydrochloride and relates to the field of medicament synthesis. According to the method, the traditional process is improved. The fasudil hydrochloride is prepared by protecting homopiperazine with di-tert-butyl dicarbonate to generate 1-Boc-homopiperazine and then reacting the 1-Boc-homopiperazine with isoquinolin-5-sulphonyl chloride. The improvement can greatly improve the reaction yield, simultaneously avoid the use of first kind or second kind of solvent and benefit the safety production and the industrial production.

The invention belongs to chemical equipment, in particular to rectification equipment which is used for recovering butyl dicarbonate in crystallized mother liquor. The rectification device comprises a column kettle, a circulating pump, a falling film type reboiler, a pylon, a condenser and a receiving tank. The invention has the advantages of high recovery rate and high product purity of butyl dicarbonate, is especially suitable for recovering butyl dicarbonate in the crystallized mother liquor, improves work efficiency and lowers production cost.

The invention relates to ten amide arylpiperazine derivatives, their preparation method, and their use in the preparation of benign prostatic hyperplasia treatment medicines. The preparation method of the amide arylpiperazine derivatives comprises the following steps: reacting free alkali of 3-bromopropylamine hydrobromide with di-tert-butyl dicarbonate to obtain a colorless oily liquid, reacting the colorless oily liquid with o-methoxyphenylpiperazine to obtain a light yellow oily material, reacting the light yellow oily material with trifluoroacetic acid to obtain a product, and reacting the product with N,N-diisopropylethylaine, 2-(7-azobenzotriazol)-N,N,N',N'-tetramethylformamidinium hexafluorophosphate, and 5-indoleacetic acid or 3-indoleacetic acid or 3-indolepropionic acid or 3-indolebutyric acid or 5-hydroxy-2-indoleacetic acid or 5-methoxy-2-indoleacetic acid or 1-methyl-3-indoleacetic acid or 6-bromo-2-indoleacetic acid or 5-chloro-2-indoleacetic acid or 7-nitro-2-indoleacetic acid to obtain final products. Experiments prove that the benign prostatic hyperplasia resistance activities of eight compounds in the amide arylpiperazine derivatives are stronger than a contrast drug prazosin.

The invention discloses a preparation method for 5-benzyl-7(S)-t-butyloxycarborylamino-5-aza-spiro[2,4]heptane. The method comprises the following steps: reacting benzoylamide acetoacetate as a raw material with 1,2-dichloroethane to obtain 3-cyclopropyl benzoylamide acetoacetate, brominating 3-cyclopropyl benzoylamide acetoacetate by NBS (n-bromosuccinimide) to obtain 1-bromo-3-cyclopropyl benzoylamide acetoacetate, cyclizing under alkaline conditions to obtain 5-benzyl-5-aza-spiro[2,4]heptane-4,7-diketone, further reacting with hydroxylamine hydrochloride to form an oxime compound-4-oxo-5-benzyl-7-oximido-5-aza-spiro[2,4]heptane, reducing by NaBH4 and boron trifluoride diethyl etherate to obtain 5-benzyl-7-amino-5-aza-spiro[2,4]heptane, performing chiral resolution by a resolving agent-L-camphorsulfonic acid to obtain 5-benzyl-7(S)-amino-5-aza-spiro[2,4]heptane, and reacting with di-tert-butyl dicarbonate ester to obtain 5-benzyl-7(S)-t-butyloxycarborylamino-5-aza-spiro[2,4]heptane. According to the method, an intermediate body-carbonyl does not need protection, raw materials are easy to get, a process route is simple, and the method is suitable for industrial production.

The invention relates to a preparation method for primary amine modified carbon nano-tubes (CNT). Firstly, the carbon nano-tubes (CNT) with carboxyl at surface are obtained after acid treatment of the carbon nano-tubes (CNT). Carboxyl carbon nano-tubes (CNT), di-tert-butyl dicarbonate and sodium azide are reacted under the composite catalysis of phase-transfer metal catalyst and Lewis acid to obtain the carbon nano-tubes (CNT) with carbamic tert-butyl. Then the tert-butyl group is lost in hydrochloric ethyl acetate solution to generate the carbon nano-tubes (CNT) with primary amine group. Compared with other methods, the carbon nano-tubes (CNT) prepared with the invention has higher primary amine level, and can be used as an important reaction intermediate as well as be compounded with polymers to obtain composite materials with high performance.

The invention relates to a method for preparing isepamicin for medicinal purpose, which comprises the following steps: (i) performing chelation reaction of gentamicin B and soluble inorganic zinc salt, and performing the amidation reaction of the product of the chelation reaction and butyl dicarbonate to form 3,6'-dibutyloxyacyl gentamicin B; (ii) performing the condensation reaction of the 3,6'-dibutyloxyacyl gentamicin B and nitrogen protected (S)-isoserine to form nitrogen protected isepamicin; and (iii) the removing the nitrogen protective group from the nitrogen protected isepamicin to form isepamicin. The invention also relates to a method for preparing isepamicin salts. The method of the invention has the advantages of high selectivity, high yield, low cost, simple operation, easy industrialization and the like.

The invention relates to a new synthetic method of a PET imaging agent L-5-<18>FETP. The method comprises the following steps: (a) carrying out a reaction between 5-hydroxytryptophan and C<1-3>alkylolto obtain a product; carrying out a reaction between the product and di-tert-butyl (i.e. (BOC)2O) to obtain N-BOC-L-5-hydroxytryptophan; (b) fluorizating 1,2-glycol tosylate in the presence of the ions such as potassium carbonate, Kryptate2.2.2 and <18>F<-> to obtain 2-<18F>-fluoroethanol p-toluene sulphonic acid ester (i.e. <18>FCH2CH2OTs); (c) carrying out a reaction between the 2-<18F>-fluoroethanol p-toluene sulphonic acid ester and the alkali metal salt of the N-BOC-L-5-hydroxytryptophan (such as sodium salt) to obtain O-(2-<18F>fluoroethyl)-N-BOC-L-5-hydroxytryptophan; (d) hydrolyzing the O-(2-<18F>fluoroethyl)-N-BOC-L-5-hydroxytryptophan under acidic conditions to remove an amino group and a carboxy protective group and obtain a final product of O-(2-<18F>fluoroethyl)-N-BOC-L-5-hydroxy tryptophan; and (e) purifying the product. The method greatly improves the radiochemical yield, obtains a sufficient quantity of a target product and realizes the clinical application of the target product.

The invention provides a new Vilanterol intermediate compound 2. According to the invention, primary amino is introduced into a compound 5 through Delepine reaction, then di-tert-butyl dicarbonate is employed for amino protection, and the strategy greatly improves the yield and atom utilization rate. On the other hand, cheap and easily available urotropin is adopted in the invention to lower the cost, thus being easy for industrial large-scale production. Compared with the prior art, the yield of the method involved in the invention is increased to 65% by three-step reaction, also use of expensive di-tert-butyl iminodicarboxylate and cesium carbonate is avoided, the cost is reduced, the operation is simple, and the conditions are mild. Therefore, the method is suitable for industrial preparation of Vilanterol and its key intermediate (5R)-5-(2, 2-dimethyl-4H-1, 3-benzodioxin-6-yl)-1, 3 oxazolidine-2-one. (formula of compound 2).

The present invention belongs to the field of chemical synthesis, relates to PET image developer preparing technology, and is especially the synthesis process of 4-acetoxyl piperidine (P4A) hydrochloride. The present invention adopts 4-hydroxyl piperidine hydrochloride as main material, pyrocarbonic acid di-tert-butyl ester in homogeneous alkaline reaction system for amino radical protection and acetic anhydride to acetylate hydroxyl radical before eliminating protecting radical, and introduces dry hydrogen chloride gas into anhydrous ethyl ether to obtain 4-acetoxyl piperidine (P4A) hydrochloride as the destination product. The process has high destination product yield of 71 %, mild reaction condition and simple operation.

The invention discloses a merariveron preparation method which includes the following steps that a, amino protection is carried out, aminobenzyl cyanide and di-tert-butyl dicarbonate react and protect para-position amine to obtain Boc aminobenzyl cyanide; b, nitrile reduction is carried out, hydrogen reduction nitrile is added to the Boc aminobenzyl cyanide under the action of a reduction catalyst of raney nickel or palladium on carbon, and Boc 2-(4-aminophenyl)ethylamine is obtained; c, condensation reaction is carried out, (R)-styrene oxide and the Boc 2-(4-aminophenyl)ethylamine react to obtain (R)-2-((4-Boc amine phenethyl) amine)-1-phenylethanol; d, deprotection is conducted, Boc groups are removed from the (R)-2-((4-Boc amine phenethyl) amine)-1-phenylethanol under the action of trifluoroacetic acid, and (R)-2-((4-amine phenethyl) amine)-1-phenylethanol is obtained; e, ester-amide condensation is carried out, the (R)-2-((4-amine phenethyl) amine)-1-phenylethanol and 2-aminothiazole-4-acetic acid are condensed under the action of a coupling reagent to obtain a target product of merariveron. The method is easy to operate and implement, raw materials are cheap and easy to obtain, reaction efficiency is high, byproducts are few, and repeatability is good.