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
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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,

Method used

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

Examples

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Example Embodiment

[0015] Example 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 sodium borohydride solution;

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

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

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

[0020] (5) Extract the wat...

Example Embodiment

[0022] Example 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 in an Erlenmeyer flask, add 40ml of absolute ethanol to dissolve it completely, and obtain 0.25mol of ethyl 4-chloroacetoacetate solution;

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

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

[0027] (5) Extract the water layer 2...

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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

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Application Information

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IPC IPC(8): C07C69/675C07C67/31
Inventor 邢将军张新荣邢晓飞
Owner NANTONG CHENGXIN AMINO ACID
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