A kind of α-acetyl-γ-butyrolactone sodium salt free acetamidine hydrochloride process

A technology of acetamidine hydrochloride and butyrolactone, which is applied in the direction of organic chemistry and the like, can solve the problems of complex preparation process of α-acetyl-γ-butyrolactone, low income, environmental pollution and the like, so as to reduce the synthesis cost and improve the benefit. , the effect of reducing production costs

Active Publication Date: 2020-08-04
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] That is to say, the preparation process of the existing α-acetyl-γ-butyrolactone is relatively complicated, and there is a large pollution to the environment, and the income is low

Method used

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  • A kind of α-acetyl-γ-butyrolactone sodium salt free acetamidine hydrochloride process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] A kind of α-acetyl-γ-butyrolactone sodium salt free acetamidine hydrochloride process, the steps are as follows:

[0066] Add 73g of α-acetyl-γ-butyrolactone sodium salt and 50g of methanol into the three-necked flask, mix at room temperature, add 50g of acetamidine hydrochloride (content 92%), and control the temperature at 10-20°C for 2 hours;

[0067] After freeing, filter to obtain 28.5g of sodium chloride;

[0068] Control the temperature of the filtrate at 30-40°C for negative pressure distillation to recover methanol to obtain 94.5 g of distillate;

[0069] 120 g of dichloromethane was added to the distillate for extraction, and the dichloromethane was added twice in equal volumes to finally obtain 27.9 g of acetamidine liquid in the upper oil layer, and the yield of acetamidine was 98.8%;

[0070] The lower oil layer is dichloromethane and α-acetyl-γ-butyrolactone;

[0071] The lower oil layer was distilled at 50-60°C under normal pressure to recover dichlorom...

Embodiment 2

[0074] A kind of α-acetyl-γ-butyrolactone sodium salt free acetamidine hydrochloride process, the steps are as follows:

[0075] Add 73g of α-acetyl-γ-butyrolactone sodium salt and 50g of methanol into the three-necked flask, mix at room temperature, add 50g of acetamidine hydrochloride (content 92%), and control the temperature at 20-30°C for 2 hours;

[0076] After freeing, filter to obtain 26.2g of sodium chloride;

[0077] Control the temperature of the filtrate at 30-40°C for negative pressure distillation to recover methanol to obtain 96.5 g of distillate;

[0078] 120 g of dichloromethane was added to the distillate for extraction, and the dichloromethane was added twice in equal volumes to finally obtain 26.3 g of acetamidine liquid in the upper oil layer, and the yield of acetamidine was 93.13%;

[0079] The lower oil layer is dichloromethane and α-acetyl-γ-butyrolactone;

[0080] The lower oil layer was distilled at 50-60°C under normal pressure to recover dichloro...

Embodiment 3

[0083] A kind of α-acetyl-γ-butyrolactone sodium salt free acetamidine hydrochloride process, the steps are as follows:

[0084] Add 73g of α-acetyl-γ-butyrolactone sodium salt and 50g of methanol into the three-necked flask, mix at room temperature, add 50g of acetamidine hydrochloride (content 92%), and control the temperature at 30-40°C for 2 hours;

[0085] After freeing, filter to obtain 25.3g of sodium chloride;

[0086] Control the temperature of the filtrate at 30-40°C for negative pressure distillation to recover methanol and obtain 97.1 g of distillate;

[0087] 120 g of dichloromethane was added to the distillate for extraction, and the dichloromethane was added twice in equal volumes to finally obtain 25.3 g of acetamidine liquid in the upper oil layer, and the yield of acetamidine was 89.59%;

[0088] The lower oil layer is dichloromethane and α-acetyl-γ-butyrolactone;

[0089] The lower oil layer was distilled at 50-60°C under normal pressure to recover dichlor...

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Abstract

The invention relates to the technical field of vitamin B synthesis intermediates, in particular to a process for dissociating acetamidine hydrochloride with alpha-acetyl-gamma-butyrolactone sodium salt. The process comprises the following steps: making alpha-acetyl-gamma-butyrolactone sodium salt react with the acetamidine hydrochloride and separating products to obtain acetamidine and alpha-acetyl-gamma-butyrolactone. According to the process, the intermediate product alpha-acetyl-gamma-butyrolactone sodium salt in the synthesis step of the alpha-acetyl-gamma-butyrolactone reacts with the acetamidine hydrochloride, the alpha-acetyl-gamma-butyrolactone sodium salt utilize hydrochloric acid coordinated in the acetamidine hydrochloride to achieve the effect that the alpha-acetyl-gamma-butyrolactone sodium salt produces the alpha-acetyl-gamma-butyrolactone, and the hydrochloric acid in the acetamidine hydrochloride is removed to form acetamidine. Synchronous production of two target products is achieved, the steps are saved, and the process is environmentally friendly and increases the revenue.

Description

technical field [0001] The invention relates to the technical field of vitamin B synthesis intermediates, in particular to a process for free acetamidine hydrochloride of α-acetyl-γ-butyrolactone sodium salt. Background technique [0002] Regarding the preparation of α-acetyl-γ-butyrolactone, there are many disclosures in the prior art, as follows: [0003] α-acetyl-γ-butyrolactone: Diketene and ethanol are acylated under the catalysis of sodium ethoxide to form ethyl acetoacetate, and then condensed with ethylene oxide and sodium hydroxide to form α-acetyl-γ-butyrolactone Lactone sodium salt, and then acidified with hydrochloric acid to obtain the crude product, which can be used as a pharmaceutical intermediate through benzene extraction and distillation. It is an important raw material for the synthesis of vitamin B. [0004] The application number is 201810135352.6, which discloses a preparation method of α-acetyl-γ-butyrolactone, which includes the following steps: un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33C07C257/14
CPCC07C257/14C07D307/33
Inventor 陈英明徐晓海李褦成严建斌崔胜凯
Owner 江苏兄弟维生素有限公司
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