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Preparation method of N,N-diisopropylethylamine

A technology of diisopropylethylamine and diisopropylamine, applied in the N field, can solve the problems of high toxicity of diethyl sulfate, environmental pollution, etc., and achieve the advantages of reducing the burden of three wastes treatment, reducing costs, and reducing harm to the environment and human body. Effect

Inactive Publication Date: 2010-06-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, diethyl sulfate is highly toxic, and large-scale use causes serious environmental pollution.

Method used

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  • Preparation method of N,N-diisopropylethylamine
  • Preparation method of N,N-diisopropylethylamine
  • Preparation method of N,N-diisopropylethylamine

Examples

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Embodiment 1

[0017] Embodiment 1, a kind of preparation method of N, N-diisopropylethylamine, take diisopropylamine and ethyl chloride as starting raw material, carry out the following steps successively:

[0018] Add 84 ml (0.6 mol) of diisopropylamine, 20.0 g (0.3 mol) of ethyl chloride, and 2 g of KI into an autoclave with a stirring temperature measuring device, and close the lid of the autoclave. use N 2 After leak detection and replacement several times, the temperature was raised to 130°C and the pressure was 0.8MPa. After maintaining the temperature for 10 h, the pressure of the autoclave no longer dropped, and the reaction was terminated.

[0019] Add saturated NaOH solution to the obtained reaction solution until PH = 13, separate the organic phase (located on the upper layer) and carry out batch rectification at atmospheric pressure, collect fractions at 127.5-128.0°C, and obtain the product N, N-diisopropylethylamine 30.4 g, the yield is 78.5%, and the structure of the obtain...

Embodiment 2

[0020] Embodiment 2, a kind of preparation method of N, N-diisopropylethylamine, take diisopropylamine and ethyl chloride as starting raw material, carry out the following steps successively:

[0021] Add 84 ml (0.6 mol) of diisopropylamine, 20.0 g (0.3 mol) of ethyl chloride, and 2 g of NaI into a high-pressure reaction kettle with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After leak detection and replacement several times, the temperature was raised to 150°C and the pressure was 1.0MPa. After maintaining the temperature for 8 hours, the pressure of the autoclave no longer dropped, and the reaction was terminated.

[0022] Add KOH solution to the resulting reaction solution until PH = 13, separate the organic phase and carry out batch rectification at atmospheric pressure, collect fractions at 127.5 to 128.0 ° C to obtain 31.3 g of the product N, N-diisopropylethylamine, and the yield is 80.6%, the structure of the obtained product wa...

Embodiment 3

[0023] Embodiment 3, a kind of preparation method of N,N-diisopropylethylamine, take diisopropylamine and ethyl chloride as starting raw material, carry out the following steps successively:

[0024] Add 127ml (0.9mol) of diisopropylamine, 20.0g (0.3mol) of ethyl chloride, CaI 2 1.5g, close the kettle lid. After leak detection and replacement with N2 several times, the temperature was raised to 150°C and the pressure was 1.2MPa. After maintaining the temperature for 8 hours, the pressure of the autoclave no longer dropped, and the reaction was terminated.

[0025] Add NaOH solution to the resulting reaction solution until PH = 13, separate the organic phase and carry out batch rectification at atmospheric pressure, collect fractions at 127.5 to 128.0°C to obtain 32.3 g of the product N,N-diisopropylethylamine, and the yield is 83.4%, the structure of the obtained product was confirmed by infrared spectroscopy.

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Abstract

The invention discloses a preparation method of N,N-diisopropylethylamine, which comprises the following steps of: reacting diisopropylamine and ethyl chloride as raw materials in a high-pressure autoclave by adopting an MIX type catalyst, wherein the mol ratio of the diisopropylamine to the ethyl chloride is 2-4:1, the mass ratio of the MIX type catalyst to the ethyl chloride is 1:20-10, the reaction temperature is 130-230 DEG C, the reaction pressure is 0.8-2.5MPa, and the reaction time is 4-10 hours; and adding a strongly alkaline solution into the obtained reaction liquid until the pH is 12.5-13.5, and then carrying out liquid separation and rectification to obtain the N,N-diisopropylethylamine. The preparation method of the N,N-diisopropylethylamine has the characteristics of simple process, high yield, low cost and little discharge of the three wastes.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing N,N-diisopropylethylamine. Background technique [0002] N, N-diisopropyl ethylamine (N, N-diisopropyl ethylamine, referred to as DIPEA) is an important organic chemical intermediate, its main use has the following aspects: (1) important pharmaceutical and pesticide intermediates, available To manufacture pharmaceutical anesthetics, pesticides and herbicides, etc. (2) Used as a condensation agent, such as for amines, CO 2 In the reaction of condensing with halogenated hydrocarbons to form urethane. (3) As a catalyst, such as a catalyst for ester hydrolysis under high pressure; used as a catalyst in the hydrolysis or condensation of phenylchloroformic acid. [0003] According to comprehensive literature reports, there are currently three main synthetic methods for N, N-diisopropylethylamine: (1) DIPEA is generated by the reaction of diisop...

Claims

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Application Information

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IPC IPC(8): C07C211/08C07C209/08
Inventor 陈新志罗虎钱超周少东
Owner ZHEJIANG UNIV
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