A kind of method for preparing alkyl acetylenic amine

Abstract

The invention discloses a method for preparing alkyl alkyne amines, which comprises the following steps: the reaction materials ammonia gas, ammonia water and alkyl alkyne chloride enter the reaction system continuously from the stirring tank I at the same time; Ⅰ, Ⅱ, Ⅲ enter the reaction system continuously; alkyl alkyne chloride reacts with ammonia to convert into alkyl acetylenic amine; the reaction mixture is layered in the separator, the alkyl acetylenic amine flows out continuously from the upper part of the separator, and ammonia water continuously flows from the lower part of the separator Outflow, through the circulating pump, a part returns to the stirring tank I, and the rest enters the ammonia desorption tower to recover ammonia, and the recovered ammonia returns to the stirring tank I. The turbine agitator used in the present invention has high shear performance and can effectively Disperse gas-liquid-liquid heterogeneous materials and promote the rapid dissolution of ammonia gas. The open-type flap turbine agitators equipped with stirred tanks II and III can effectively disperse liquid-liquid heterogeneous materials. They have high ammonia concentration, alkane It has the characteristics of low concentration of alkyne chloride and low concentration of sodium hydroxide, which can effectively inhibit side reactions and improve reaction selectivity.

Description

technical field [0001] The present invention relates to a method for preparing alkyl acetylenic amines. Background technique [0002] The reaction for preparing alkylalkynylamines from alkylalkyne chlorides is shown in the following formula: [0003] In the formula, R=CH 3 、C 2 h 5 . [0004] Alkynylamines are important intermediates for the preparation of medicines and pesticides. For example 3-amino-3-methyl-1-butyne (R=CH 3 ) is an important intermediate for the preparation of the herbicide propyzamide. 3-Amino-3-methyl-1-pentyne (R=C 2 h 5 ) is an important intermediate for the preparation of the fungicide zoxamide. [0005] The document US6087535 reports a method for preparing alkyl alkyne amines from alkyl alkyne chlorides: at -33°C, 50% sodium hydroxide solution is added dropwise to a mixture of liquid ammonia and alkyl alkyne chlorides. After the reaction was completed, the ammonia was evaporated, and water was added to separate the layers. The method ha...

AI Technical Summary

Problems solved by technology

This method has following defects: need to use autoclave; Low temperature operation; Residual ammonia of reaction is difficult to recycle; Intermittent operation, production capacity is small

This method has following defect: because reaction has water to produce, there is water in the sodium hydroxide solution of dripping, and reaction consumes ammonia, these cause the ammoniacal liquor concentration of late stage of reaction to be more and more low, and side reaction (mainly generates alkyl alkyne alcohol and alkyl alkyne Secondary amine) more and more, the yield is low (yield is only 57%); Residual ammonia water is difficult to recycle; Intermittent operation, reaction time is long, production capacity is small

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