Supercharge Your Innovation With Domain-Expert AI Agents!

Synthesis process of chloroacetic anhydride

A technology for the synthesis of chloroacetic anhydride, which is applied in the field of synthesis of chloroacetic anhydride, can solve the problems of equipment corrosion, strong corrosion of equipment, and high requirements for equipment, and achieve the goals of less equipment investment, good product quality, and reduced process energy consumption Effect

Inactive Publication Date: 2018-06-22
上海仁实医药科技有限公司
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When the above-mentioned patented product chloroacetic anhydride is synthesized, firstly, hydrogen chloride gas will be produced as a by-product, which is highly corrosive to equipment; secondly, the process uses high-temperature heating and high-vacuum systems for a long time; overall, the process requires High temperature, high vacuum conditions are required, and it is easy to corrode the equipment

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthesis process of chloroacetic anhydride
  • Synthesis process of chloroacetic anhydride
  • Synthesis process of chloroacetic anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: a kind of synthetic technique of chloroacetic anhydride, comprises the following steps:

[0027] Step 1, preparation of chloroacetic anhydride solution: add 1 equivalent of sodium chloroacetate to the reaction flask, then add an aprotic solvent, the weight of the aprotic solvent is twice that of sodium chloroacetate, heat to 40°C, stir, and slowly drop 0.9 equivalents of chloroacetyl chloride, after 2 hours of dropwise addition, continue to stir at 40°C for 1 hour, filter, filter the filter cake after washing with an aprotic solvent, and combine the filtrates to obtain a chloroacetic anhydride solution with a purity of 95%. The rate is 95%, wherein the aprotic solvent is toluene;

[0028] Step 2, purification of chloroacetic anhydride: add the above-mentioned chloroacetic anhydride solution into the reactor, add petroleum ether, cool to 35°C, continue stirring until the solid precipitates, cool down to 0°C, keep stirring for 1 hour, filter, and use for fil...

Embodiment 2

[0031] Embodiment 2: a kind of synthetic technique of chloroacetic anhydride, the difference with embodiment one is, comprise the following steps: step 1, the preparation of chloroacetic anhydride solution: add 1 equivalent sodium chloroacetate in reaction bottle, then add Aprotic solvent, the weight of the aprotic solvent is 3 times that of sodium chloroacetate, heated to 40 ° C, stirred, slowly added dropwise 1 equivalent of chloroacetyl chloride, after 2 hours, the addition was completed, and continued to stir at 40 ° C for 1 hour, Filtration, the filter cake was washed with an aprotic solvent and filtered, and the filtrates were combined to obtain a chloroacetic anhydride solution with a purity of 95% and a yield of 95.1%, wherein the aprotic solvent was toluene;

[0032] Step 2, purification of chloroacetic anhydride: add the above-mentioned chloroacetic anhydride solution into the reactor, add petroleum ether, cool to 35°C, continue stirring until the solid precipitates, ...

Embodiment 3

[0033] Embodiment 3: a kind of synthetic technique of chloroacetic anhydride, differs from embodiment one in, comprises the following steps: Step 1, the preparation of chloroacetic anhydride solution: add 1 equivalent sodium chloroacetate in reaction bottle, then add Aprotic solvent, the weight of the aprotic solvent is 5 times that of sodium chloroacetate, heated to 40 ° C, stirred, slowly added dropwise 1.2 equivalents of chloroacetyl chloride, after 2 hours, the addition was completed, and continued to stir at 40 ° C for 1 hour, Filtration, the filter cake was washed with an aprotic solvent and filtered, and the filtrates were combined to obtain a chloroacetic anhydride solution with a purity of 95.1% and a yield of 95.3%, wherein the aprotic solvent was toluene;

[0034] Step 2, purification of chloroacetic anhydride: add the above-mentioned chloroacetic anhydride solution into the reactor, add petroleum ether, cool to 35°C, continue stirring until the solid precipitates, c...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a synthesis process of chloroacetic anhydride, and relates to the technical field of medicine synthesis. The problems that the existing process can easily generate corrosion onthe equipment, and the high-temperature and high-vacuum conditions are needed are solved. The process comprises the following steps of chloroacetic anhydride solution preparation: dripping sodium chloroacetate and aprotic solvents into a reaction bottle; performing heating to 40 to 50 DEG C; performing stirring; slowly dripping chloroacetyl chloride; completing the dripping in 2 to 3 hours; continuously performing stirring for 1 to 2 hours under the condition of 40 to 50 DEG C; performing filtering; washing filter cake with aprotic solvents; performing filtering; merging filter liquid to obtain a chloroacetic anhydride solution; purifying the chloroacetic anhydride; adding the chloroacetic anhydride solution into a reactor; adding petroleum ether; performing cooling to 35 to 40 DEG C; continuously performing stilling until solid is separated out; lowering the temperature to 0 to 5 DEG C; performing heat insulation stirring for 1 to 2 hours; performing filtering; washing the filter cake with petroleum ether; drying the filter cake to obtain white crystal solid products which are chloroacetic anhydride. The process has the advantages that hydrogen chloride gas is not generated; theanti-corrosion requirement on the equipment is low; the reaction conditions are mild; the energy consumption is reduced.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical synthesis, more specifically, it relates to a synthesis process of chloroacetic anhydride. Background technique [0002] Chloroacetic anhydride is a chemical reagent widely used in pesticide, medicine, chemical industry and other industries. Chloroacetic anhydride is also a very important pharmaceutical intermediate, which can be used to prepare various drugs containing esters, amides and other structures. [0003] The Chinese invention patent with publication number CN101823947A discloses a synthesis process of chloroacetic anhydride, which reacts with chloroacetic acid and chloroacetyl chloride as raw materials, and its molar ratio is: chloroacetyl chloride: and chloroacetic acid=1:1~ 5; The operation steps are: (1), add chloroacetic acid into the four-necked flask, cool down to 10-15°C, add chloroacetyl chloride; (2), slowly heat the reaction to 40-50°C, when gas is released, keep warm ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/56C07C51/573C07C53/15
CPCC07C51/56C07C51/573C07C53/15
Inventor 李文杰宋东林长学
Owner 上海仁实医药科技有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com