Synthesis method of N-methyl-2-hydroxyethyl hydroxyethyl

Abstract

The invention discloses a synthesis method of N-methyl-2-hydroxyethyl hydroxyethyl, which comprises the following steps of: (1) adding dimethyl sulfate and N-methyl pyrrolidone into a reaction kettle for reaction; (2) cooling and dropwise adding an ethanol solution of sodium ethylate, continuously dropwise adding ethyl cyanoacetate, reacting and filtering to obtain an intermediate (I); (3) adding the intermediate (I) and a catalyst as well as a high-boiling point organic solvent to the reaction kettle, heating, fractionating, reacting, filtering, recovering propylene glycol, and carrying vacuum rectification to obtain a intermediate (II); and (4) adding the intermediate (II) and the catalyst as well as a solvent into the reaction kettle, replacing by using nitrogen and hydrogen sequentially, introducing hydrogen, reacting, cooling, evacuating, filtering, evaporating out moisture content, and carrying out vacuum rectification to obtain the N-methyl-2-hydroxyethyl hydroxyethyl. The synthesis method has the advantages of cheap and easily obtained raw materials, short synthesis route, mild reaction conditions, relatively low production cost and higher overall yield.

Description

technical field [0001] The invention relates to a synthesis method of pyrrolidine, in particular to a synthesis method of N-methyl-2-hydroxyethylpyrrolidine, and belongs to the field of synthesis of pyrrolidine. Background technique [0002] N-methyl-2-hydroxyethylpyrrolidine is a colorless and transparent liquid with amino compounds, which is mainly used in the preparation of antipsychotic and antiviral drugs. [0003] Mainly disclose the synthetic routes of A, B and C total 3 kinds of N-methyl-2-(β-hydroxyethyl) pyrrolidines in the prior art (see figure 1 , figure 2 with image 3 ). In the above three synthetic routes, side chain reaction is involved, which is their common point and the core of synthesizing the subject compound. The side chain reaction of vinyl acetate on the pyrrolidine ring or pyrrolidone ring is a typical free radical addition reaction, and the yields are: route A: 86%, route B: 78%, route C: 67%. For C, due to the N-CH 3 A similar reaction can t...

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to overcome the problems of high production cost and low yield in the existing synthetic method of N-methyl-2-hydroxyethylpyrrolidine, and provide a new N-methyl-2-hydroxyethylpyrrolidine - a synthetic method for 2-hydroxyethylpyrrolidine, which has the advantages of simple and convenient steps, lower production cost and high yield

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