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Synthesis method of diethyl acetamidomalonate

A technology of diethyl acetamidomalonate and diethyl malonate, which is applied in chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve problems such as difficulty in improving yield, and achieve production rate-enhancing effect

Active Publication Date: 2021-07-16
湖北宇阳药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of synthetic method of diethyl acetamidomalonate, which is used to solve the problem that the yield of the synthetic method of diethyl acetamidomalonate is difficult to improve in the prior art

Method used

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Examples

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Effect test

preparation example Construction

[0012] The step of the synthetic method of acetamidodiethyl malonate in the present invention comprises:

[0013] (1) Add glacial acetic acid and sodium nitrite solution into diethyl malonate successively, keep warm for reaction, and take the oil layer solution after standing for stratification. In this step, specifically, add glacial acetic acid to diethyl malonate in an ice bath environment, keep the temperature at 3-5°C, gradually add sodium nitrite solution dropwise, and control the dropping process through the ice bath environment The temperature is not higher than 10°C. After the dropwise addition, remove the ice bath environment, and keep it warm at 30-40°C for 3-4 hours to obtain the reaction liquid. The waste gas generated during the reaction can be discharged from the fume hood; the reaction liquid is left to stand and stratified. , and extract the oil layer solution; wherein, the mass ratio of sodium nitrite and glacial acetic acid contained in diethyl malonate and ...

Embodiment 1

[0019] The specific steps of synthesizing diethyl acetamidomalonate in the present embodiment are as follows:

[0020] (1) Get the there-necked flask and add 25g of diethyl malonate, cool in an ice bath, add 33g of glacial acetic acid, add dropwise 44% sodium nitrite solution when the temperature drops to 5°C (this sodium nitrite solution consists of 32.5g of sodium nitrite Dissolved in 40.5g water to prepare), during the dropping process, control the temperature not higher than 10°C, after the dropwise addition, remove the water bath environment, keep warm at 30-40°C, continue to stir for 4 hours, the NO produced in the reaction should be covered with a fume hood Discharge; after the reaction is completed, the reaction solution is statically layered in a separatory funnel, and the oil layer solution is taken.

[0021] (2) Pour 18.7g of the oil layer solution into another three-necked flask, add 118g of acetic acid, add 35g of potassium borohydride and 78g of methanol solution...

Embodiment 2

[0024] The specific steps of synthesizing diethyl acetamidomalonate in the present embodiment are as follows:

[0025] (1) Get a three-necked flask and add 25g of diethyl malonate, cool in an ice bath, add 35g of glacial acetic acid, add dropwise 44% sodium nitrite solution when the temperature drops to 5°C (this sodium nitrite solution consists of 32.5g of sodium nitrite Dissolved in 40.5g water to prepare), during the dropping process, control the temperature not higher than 10°C, after the dropwise addition, remove the water bath environment, keep warm at 30-40°C, continue to stir for 4 hours, the NO produced in the reaction should be covered with a fume hood Discharge; after the reaction is completed, the reaction solution is statically layered in a separatory funnel, and the oil layer solution is taken.

[0026] (2) Pour 18g of the oil layer solution into another three-necked flask, add 108g of acetic acid, add 33g of potassium borohydride and 72g of methanol solution in ...

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PUM

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Abstract

The invention discloses a synthesis method of diethyl acetamidomalonate, which comprises the steps of sequentially adding glacial acetic acid and a sodium nitrite solution into diethyl malonate, carrying out heat preservation reaction, standing for layering, and taking an oil layer solution; and sequentially adding glacial acetic acid, potassium borohydride, methanol and acetic anhydride into the oil layer solution, stirring to react, washing, and distilling to obtain the diethyl acetamidomalonate. The potassium borohydride reducing agent is introduced, so that the yield of the diethyl acetamidomalonate obtained by the reaction is obviously improved.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing diethyl acetamidomalonate. Background technique [0002] Diethyl acetamidomalonate, also known as diethyl α-acetamidomalonate, is an important intermediate in the process of pharmaceutical synthesis. At present, diethyl acetamidomalonate is not only an important intermediate of rebamipide anti-gastrointestinal ulcer drug, but also can be used to synthesize desmethylclolincomycin hydrochloride, lincomycin, amyllincomycin It can also be used in the synthesis of α-amino acids, such as intermediates of tryptophan and Xiaotong mustard. In the prior art, the zinc powder reduction method is used to prepare diethyl acetamidomalonate, but the yield is difficult to reach more than 90%, so a new synthetic scheme needs to be proposed to solve the problem of acetamidomalonate in the prior art. Diethyl acid yield is difficult to improve the problem. Contents of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/47C07C231/12
CPCC07C231/12C07C233/47
Inventor 陈挺钱坚锋刘成黄小庭余依玲王正豪
Owner 湖北宇阳药业有限公司
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