Synthesis method of N, N-diisopropylethylamine

Abstract

The invention discloses a synthesis method of N, N-diisopropylethylamine. The synthesis method comprises the following steps of: (1) reacting paraldehyde serving as a raw material in a solvent under normal pressure and at the temperature of 22-28 DEG C under the action of an acidic catalyst for 20-40 minutes; (2) adding diisopropylamine and metal hydride serving as a reducing agent into a reaction product obtained by the step (1), preserving heat and reacting for 10-30 minutes to obtain the N, N-diisopropylethylamine, wherein the molar ratio of the diisopropylamine to the paraldehyde is 1:0.34-0.4, the molar ratio of the diisopropylamine to the metal hydride is 1:1-1.2, and the mass ratio of the acidic catalyst to the diisopropylamine is 1-5 percent; and (3) after removing the solvent under reduced pressure from reaction solution obtained by the step (2), adjusting pH (Potential of Hydrogen) to be 13, and then separating and rectifying to obtain the N, N-diisopropylethylamine.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing N,N-diisopropylethylamine (DIPEA for short). Background technique [0002] N,N-Diisopropylethylamine is an important organic chemical intermediate, which is mainly used in the following aspects: (1) an important pharmaceutical and pesticide synthesis intermediate; (2) can also be used as a condensation Mixing agent, such as for the condensation of carbon monoxide, amine and alkyl halide to form urethane; (3) As a catalyst for ester hydrolysis and other reactions. [0003] According to comprehensive literature reports, there are currently three main synthetic methods for N,N-diisopropylethylamine: [0004] 1) Patent CN101759571 reports a method to generate DIPEA by reacting diisopropylamine and alkyl halide, the reaction pressure is 0.4~2.5MPa, and the yield is about 95%. However, the reaction generates salt, which requires high equipment s...

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Problems solved by technology

However, the reaction generates salt, which requires high equipment stirring, and the reaction generates hydrogen halide, which is corrosive to the equipment;

[0005] 2) In the document "Synthesis of N,N-diisopropylethylamine", a method for synthesizing DIPEA using diisopropylamine and diethyl sulfate as raw materials was reported, with a yield of 90% and a simple process, which is currently the most The commonly used route, but diethyl sulfate is more toxic and seriously pollutes the environment;

However, the reaction pressure of this method is high, the catalyst is expensive, and the yield is also low.