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Improved method for hydrolysis process in preparation process of L-phenylglycinol

A preparation process and technology of phenylglycinol, which are applied in the preparation of amino hydroxy compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as difficult control of hydrolysis temperature, and achieve the effect of improving reaction safety and product quality.

Inactive Publication Date: 2018-09-04
NANTONG WANNIANCHANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problem that the hydrolysis temperature is difficult to control in the preparation process of L-phenylglycine, and provides a method for improving the hydrolysis process in the preparation process of L-phenylglycine, which can control the hydrolysis temperature within a safe range, thereby Greatly improved reaction safety and product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 170kg of sodium borohydride and 260kg of L-phenylglycine were put into the reactor, cooled down, and 800kg of tetrahydrofuran was added. Slowly add 250kg of concentrated sulfuric acid dropwise. After the drop is completed, keep the temperature for about 2-3 hours. During the dropwise addition, the temperature must be strictly controlled. After the heat preservation is over, slowly turn on the steam atmospheric pressure distillation to recover THF. After observing that the concentrated liquid in the kettle becomes thicker and the amount of THF evaporated under normal pressure is significantly reduced, then vacuum distillation (about 1h), and close it after the stirring stops automatically. Stir, concentrate to dryness, cool down and vent. Slowly add 400kg of ice-water mixture at 0°C that has been cooled with a cooling kettle in advance, and increase the amount of water after the water has soaked into the material, and then add dropwise 400kg of 20% sodium hydroxide solut...

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PUM

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Abstract

The invention discloses an improved method for a hydrolysis process in a preparation process of L-phenylglycinol. L-phenylglycine, sodium borohydride and tetrahydrofuran are put into a reaction still,sulfuric acid is added dropwise, and after the reaction is completed, tetrahydrofuran is recovered under reduced pressure; an ice-water mixture previously frozen in a cooling kettle is slowly fed into the reaction still for hydrolysis, and a sodium hydroxide solution previously frozen in the cooling kettle is slowly added into the reaction still; stirring hydrolysis is started, remaining solventsare distilled off, and toluene is added for standing and stratification; cooling and centrifugation are conducted to obtain L-phenylglycinol. The preparation process is simple and suitable for industrial production.

Description

technical field [0001] The present invention relates to a method for improving the hydrolysis process in the preparation process of L-phenylglycine, and more specifically relates to the improvement of the hydrolysis process in the process of reducing L-phenylglycine to L-phenylglycine through sodium borohydride . Background technique [0002] Asymmetric synthesis is an extremely important and dynamic research field in organic chemistry. It is increasingly used in the synthesis of natural products with complex structures and stereochemistry. Different strategies can be used to introduce new chiral units into target products. , and chiral auxiliary reagents are an effective method. Chiral oxazolidinones, originally prepared by Evans, are a class of chiral auxiliary agents developed in recent years, which have good inductive effects. [0003] Among all oxazolidinone chiral auxiliaries, (S)-4-phenyl-2-oxazolidinone is the most widely studied and the best induction effect. The...

Claims

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Application Information

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IPC IPC(8): C07C213/00C07C213/10C07C215/28
CPCC07C213/00C07C213/10C07C215/28
Inventor 李凯鲍烨华王敏姜明
Owner NANTONG WANNIANCHANG PHARMA