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Preparation method of 1-tert-butyloxycarbonyl-3-cyano-4-oxo-pyrrolidine

A technology of butoxycarbonyl and pyrrolidine, which is applied in the field of preparation of 1-tert-butoxycarbonyl-3-cyano-4-oxo-pyrrolidine, can solve the problem of high cost, complex synthesis process and difficulty in meeting market demands and other problems, to achieve the effect of low cost and easy operation

Inactive Publication Date: 2010-11-03
JIANGSU HUILILONG PLASTIC IND GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its complex synthesis process and high cost, it is difficult to meet market demand through traditional production

Method used

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  • Preparation method of 1-tert-butyloxycarbonyl-3-cyano-4-oxo-pyrrolidine
  • Preparation method of 1-tert-butyloxycarbonyl-3-cyano-4-oxo-pyrrolidine
  • Preparation method of 1-tert-butyloxycarbonyl-3-cyano-4-oxo-pyrrolidine

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Embodiment Construction

[0021] The technical features of the present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0022] see figure 2 , is the chemical reaction formula of the present invention, and its steps are:

[0023] 1) Put 168 grams of glycine ethyl ester hydrochloride and 600 mL of methanol into a 2000 mL three-neck flask, mechanically stir and dissolve. Add 48 g of NaOH solid in four times, and ice-water bath, and the slurry is white. Heat to 70°C in an oil bath, add 80g of acrylonitrile dropwise, after the dropwise addition is complete, reflux the reaction, spot the plate to track the reaction progress, PE:EA=1:5. The time is about 4 hours.

[0024] 2) After the reaction is completed, cool to room temperature, add 218g (BOC)2O (1.0mol) in 6 times within 1-2 hours, and react at room temperature, showing a white suspension. Point the plate to judge the progress of the reaction. After the reaction, filter with suction...

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Abstract

The invention provides a preparation method of 1-tert-butyloxycarbonyl-3-cyano-4-oxo-pyrrolidine, comprising the following steps: placing 168g of glycine ethyl ester hydrochloride and 600ml of methanol into a three-necked flask, stirring and dissolving to obtain clear liquid; adding 48g of NaOH solid in four times, and then carrying out ice-water bath until the obtained mixed liquid is in a white pulp shape; carrying out oil bath, heating to 70 DEG C, dropwise adding 80g of acrylonitrile, carrying out reflux reaction, and adding 218g of (BOC)2O at a room temperature in six times for 1-4h to obtain white suspension; filtering, merging filtrate, removing methanol by rotary evaporation, adding 400ml of ethyl acetate and extracting, washing with 200ml of water for three times, drying with 40g of an EA anhydrous magnesium sulfate layer, and then keeping standing; filtering the EA layer, removing a solvent EA by rotary evaporation to obtain a light yellow oily substance I; and adding 43g of NaH (70%) and 700ml of dried methylbenzene to the three-necked flask, stirring, heating reflux at about 110 DEG C, dropwise adding a raw material I for quinary cyclization reaction, layering, re-extracting, filtering and then drying to obtain the 1-tert-butyloxycarbonyl-3-cyano-4-oxo-pyrrolidine.

Description

technical field [0001] The invention relates to a pharmaceutical intermediate, and specifically discloses a preparation method of 1-tert-butoxycarbonyl-3-cyano-4-oxo-pyrrolidine. Background technique [0002] At present, various new drugs are emerging in the market, especially the synthesis of anti-tumor, anti-infection drugs and pesticides, most of which require a pharmaceutical intermediate - 1-tert-butoxycarbonyl-3-cyano-4-oxo-pyrrolidine, From the existing literature, 1-tert-butoxycarbonyl-3-cyano-4-oxo-pyrrolidine plays an extremely important role in the synthesis of anti-tumor, anti-infection and other drugs and pesticides, not only improving the quality of the compound, And because of its stability, the effective life of the composition is extended. However, due to its complex synthesis process and high cost, it is difficult to meet market demand through traditional production. Contents of the invention [0003] A preparation method of 1-tert-butoxycarbonyl-3-cyan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/24
Inventor 杜建
Owner JIANGSU HUILILONG PLASTIC IND GROUP