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Synthesis method of caronic anhydride

A synthesis method and carronic anhydride technology, applied in the direction of organic chemistry and the like, can solve the problems of high production cost and high raw material price, and achieve the effects of short reaction route, low price and simple production process

Inactive Publication Date: 2014-11-19
WUZHOU SONGHUA AROMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem that the present invention solves is to provide a kind of synthesis method of caronic anhydride, the synthetic method of this caronic anhydride can solve the problem that the raw material price used in the existing production method of caronic anhydride is relatively expensive, thereby causes its production cost too high question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The synthetic method of bencarbronic anhydride, the method comprises the following steps:

[0021] A. Put 136g of 3-carene and 1.36g of cetyl sodium sulfate into the reactor, add 2370g of water, start stirring, and control the temperature in the reactor to 5°C, add 474g of potassium permanganate to keep warm and react 15 hours; Wherein, the adding time of this potassium permanganate is controlled within 3 hours;

[0022] B. Suction filtration is performed on the material prepared by the reaction in step A, the filtrate and filter cake are collected, the filter cake is washed once with water, the washing liquid is collected, and mixed with the filtrate to obtain a mixed solution;

[0023] C. Adjust the pH value of the mixed solution prepared in step B to 10, then extract it twice with benzene, and collect the water layer; wherein, for each extraction, the amount of benzene is 1 / 4 of the volume of the mixed solution;

[0024] D. Adjust the pH value of the water layer obt...

Embodiment 2

[0028] The synthetic method of bencarbronic anhydride, the method comprises the following steps:

[0029] A. Put 136g of 3-carene and 1.36g of cetyl sodium sulfate into the reactor, add 1580g of water, start stirring, and control the temperature in the reactor to 35°C, add 316g of potassium permanganate to keep warm and react 5 hours; Wherein, the adding time of this potassium permanganate is controlled within 3 hours;

[0030] B, carry out suction filtration with the material that A step reaction makes, collect filtrate and filter cake, wash described filter cake with water 3 times, collect washing liquid, and mix with described filtrate, make mixed solution;

[0031] C, adjusting the pH value of the mixed solution prepared in step B to 10, then extracting with benzene for 3 times, and collecting the water layer; wherein, for each extraction, the amount of benzene is 1 / 4 of the volume of the mixed solution;

[0032] D. Adjust the pH value of the water layer obtained in step ...

Embodiment 3

[0036] The synthetic method of bencarbronic anhydride, the method comprises the following steps:

[0037] A. Put 136g of 3-carene and 1.36g of cetyl sodium sulfate into the reactor, add 790g of water, start stirring, and control the temperature in the reactor to 25°C, add 158g of potassium permanganate to keep warm and react 15 hours; Wherein, the adding time of this potassium permanganate is controlled within 3 hours;

[0038] B. Suction filtration is performed on the material prepared by the reaction in step A, the filtrate and filter cake are collected, the filter cake is washed with water twice, the washing liquid is collected, and mixed with the filtrate to obtain a mixed solution;

[0039] C. Adjust the pH value of the mixed solution prepared in step B to 10, then extract it twice with benzene, and collect the water layer; wherein, for each extraction, the amount of benzene is 1 / 4 of the volume of the mixed solution;

[0040] D. Adjust the pH value of the water layer ob...

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Abstract

The invention discloses a synthesis method of caronic anhydride and belongs to the technical field of deep process of turpentine. The method includes following steps: filling a reactor with 3-carane and cetyl sodium sulfate with addition of water; performing a stirring process; adding potassium permanganate within 3 hours; carrying out a reaction with heat preservation; performing a suction filtration process; washing a filter cake with water; mixing a washed liquid and a filtrate; adjusting a pH value to 10; performing an extraction process with benzene; collecting a water layer; adjusting a pH value to 2; performing a concentrating process, a drying process, a filtering process, a washing process and a drying process; performing a mixing process with acetic anhydride and sodium acetate; carrying out a reaction; and finally adding methylbenzene and petroleum ether and performing a crystallization process to obtain the caronic anhydride. Required raw materials in the method are low in cost and the caronic anhydride is low in production cost. In addition, the method is short in reaction route and is simple in processes.

Description

technical field [0001] The invention belongs to the technical field of turpentine deep processing, and in particular relates to a synthesis method of caronic anhydride. Background technique [0002] Caronic anhydride is a pharmaceutical intermediate, mainly used for the synthesis of oral hepatitis C protease inhibitor Boceprevir. Boceprevir is an oral hepatitis C protease inhibitor developed by Schering-Plough. Its molecular structure is as follows: [0003] . [0004] At present, the synthesis method of caronic anhydride is mainly prepared from chrysanthemic acid ester through oxidation, saponification, acidification and dehydration cyclization. More expensive, resulting in high production costs. Contents of the invention [0005] The technical problem that the present invention solves is to provide a kind of synthesis method of caronic anhydride, the synthetic method of this caronic anhydride can solve the problem that the raw material price used in the existing pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/93
CPCC07D307/93
Inventor 杨韶平陈键泉刘娟娟陈伟强董俊谭育慧
Owner WUZHOU SONGHUA AROMATIC CHEM
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