Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing hydroxyl ester

A technology for the synthesis of hydroxy esters and hydroxy esters, applied in the field of preparation of hydroxy esters, can solve the problems of high cost, low purity, low yield, etc., and achieve the effect of low cost and easy reaction

Inactive Publication Date: 2012-01-04
NANTONG CHENGXIN AMINO ACID
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Hydroxyester is an important organic intermediate. In the traditional process of synthesizing hydroxyester, ethyl 4-chloro-3-carbonylbutyrate is reacted with a large amount of anhydrous methanol to obtain a methanol solution of hydroxyester, and then through distillation, Recover the solvent, wash with water to remove the inorganic salt, and finally extract and concentrate to obtain the product, which makes the cost of the synthesis method relatively high, and the reaction is difficult to control, the yield is low, and the purity is less than 80%.

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
  • Method for preparing hydroxyl ester
  • Method for preparing hydroxyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1), weigh 1.89g of sodium borohydride, add 120ml of absolute ethanol and 10ml of 1% sodium hydroxide solution to obtain 0.05mol of sodium borohydride solution;

[0017] (2), weigh 16.45 g of ethyl 4-chloroacetoacetate in a conical flask, add 30 ml of absolute ethanol to dissolve completely, and obtain 0.1 mol of ethyl 4-chloroacetoacetate solution;

[0018] (3) Add the sodium borohydride solution into a 250ml three-neck flask, add the ethyl 4-chloroacetoacetate solution dropwise into the sodium borohydride solution within 10 minutes through the dropping funnel, and place it in an ice-water bath at 0-3°C After reacting for 2 hours, use pure ethanol to neutralize to acidity, and stir to complete the reaction;

[0019] (4), filter the reaction solution to remove salt, then concentrate under reduced pressure to get ethanol, then salt out with saturated brine, separate the oil layer, and put it into another clean three-necked flask;

[0020] (5), extract the water layer wi...

Embodiment 2

[0023] (1), weigh 3.28g of sodium borohydride, add 180ml of absolute ethanol and 20ml of 1% sodium hydroxide solution to obtain 0.12mol of sodium borohydride solution;

[0024] (2), weigh 25.21 g of ethyl 4-chloroacetoacetate with a conical flask, add 40 ml of absolute ethanol to dissolve completely, and obtain 0.25mol of ethyl 4-chloroacetoacetate solution;

[0025] (3) Add the sodium borohydride solution into a 250ml three-neck flask, add the ethyl 4-chloroacetoacetate solution dropwise into the sodium borohydride solution within 20 minutes through the dropping funnel, and place it in an ice-water bath at 0-3°C After reacting for 5 hours, use pure ethanol to neutralize to acidity, and stir to complete the reaction;

[0026] (4), filter the reaction solution to remove salt, then concentrate under reduced pressure to get ethanol, then salt out with saturated brine, separate the oil layer, and put it into another clean three-necked flask;

[0027] (5), extract the water layer ...

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 provides a method for preparing hydroxyl ester. The hydroxyl ester is reduced and synthesized by taking 4-chloracetyl acetidin as a raw material and taking sodium borohydride as a reducing agent in an alkaline environment. According to the method for preparing the hydroxyl ester provided by the invention, the cost is low; the reaction is easy to control; the yield is above 80%; and the purity is above 95%.

Description

technical field [0001] The invention relates to a preparation method of hydroxy ester, which belongs to the field of pharmaceutical manufacturing. Background technique [0002] Hydroxyester is an important organic intermediate. In the traditional process of synthesizing hydroxyester, ethyl 4-chloro-3-carbonylbutyrate is reacted with a large amount of anhydrous methanol to obtain a methanol solution of hydroxyester, and then through distillation, The solvent is recovered, the inorganic salt is removed by water washing, and finally the product is obtained by extraction and concentration, which makes the synthesis method cost relatively high, and the reaction is difficult to control, the yield is low, and the purity is less than 80%. Contents of the invention [0003] In order to overcome the shortcomings of the prior art, the invention provides a preparation method of hydroxyester, which is characterized in that: in an alkaline environment, ethyl 4-chloroacetoacetate is used...

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
IPC IPC(8): C07C69/675C07C67/31
Inventor 邢将军张新荣邢晓飞
Owner NANTONG CHENGXIN AMINO ACID
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com