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Synthesis method of N,N-diethyl isopropylamine

A technology of diethylisopropylamine and a synthetic method, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems that solvents increase the difficulty of product separation, it is difficult to realize industrial production, and the price of raw materials is expensive. Achieve the effect of low price, high utilization rate of raw materials, and simple post-processing

Inactive Publication Date: 2011-09-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials of this method are expensive, the production cost is high, and the use of solvent increases the difficulty of product separation, recovery and application are difficult, while the reaction time is long, the yield is low, and there are many by-products, so it is difficult to realize industrial production.

Method used

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  • Synthesis method of N,N-diethyl isopropylamine
  • Synthesis method of N,N-diethyl isopropylamine
  • Synthesis method of N,N-diethyl isopropylamine

Examples

Experimental program
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Embodiment 1

[0027] Embodiment 1, a kind of N, N, the synthetic method of-diethylisopropylamine:

[0028] Add 58.6g (0.8mol) of diethylamine and 31.4g (0.4mol) of isopropyl chloride into the autoclave with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After checking for leaks and replacing the air several times, the temperature was raised to 100°C and the pressure was 0.2MPa. The reaction was terminated after maintaining the temperature for 4 h.

[0029] Add NaOH aqueous solution (mass concentration: 10%) to the obtained reaction product until PH = 13.5, separate the upper organic phase for rectification, collect 107.5~108.0°C fractions, and obtain the product N,N,-diethylisopropylamine 36.4g, the yield is 79.2%, the purity is 99%, and the obtained product is characterized by the correct structure.

Embodiment 2

[0030] Embodiment 2, a kind of N, N, the synthetic method of-diethylisopropylamine:

[0031] Add 58.6g (0.8mol) of diethylamine and 31.4g (0.4mol) of isopropyl chloride into the autoclave with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After checking for leaks and replacing the air several times, the temperature was raised to 150°C and the pressure was 0.6MPa. The reaction was terminated after maintaining the temperature for 6 h.

[0032] Add KOH aqueous solution (mass concentration: 20%) to the obtained reaction product until PH = 13.5, separate the organic phase located in the upper layer for rectification, collect fractions at 107.5~108.0°C, and obtain the product N,N,-diethyliso Propylamine was 37.4g, the yield was 81.2%, and the purity was 99%. The resulting product was characterized and had a correct structure.

Embodiment 3

[0033] Embodiment 3, a kind of N, N, the synthetic method of-diethylisopropylamine:

[0034] Add 58.6g (0.8mol) of diethylamine and 31.4g (0.4mol) of isopropyl chloride into the autoclave with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After checking for leaks and replacing the air several times, the temperature was raised to 140°C and the pressure was 0.5MPa. After maintaining the temperature for 8 hours, the reaction was terminated.

[0035] Add KOH aqueous solution (mass concentration: 30%) to the obtained reaction product until PH = 11.5, separate the organic phase located in the upper layer for rectification, collect fractions at 107.5~108.0°C, and obtain the product N,N,-diethyliso Propylamine was 39.3g, the yield was 85.4%, and the purity was 99%. The resulting product was characterized to have a correct structure.

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Abstract

The invention discloses a synthesis method of N,N-diethyl isopropylamine. The synthesis method comprises the following steps of: making diethylamine and isopropyl chloride serving as raw materials react in a high-pressure kettle in the absence of a solvent and a catalyst at the reaction temperature of 100-200 DEG C under the reaction pressure of 0.2-1.1 Mpa for 4-10 hours, wherein the molar ratio of the diethylamine to the isopropyl chloride is (2-5):1; and adding an inorganic alkaline solution into an obtained reaction product until the pH is 11.5-13.5, separating liquid and fractionating to obtain the N,N-diethyl isopropylamine. The synthesis method of N,N-diethyl isopropylamine has the characteristics of environmental friendliness, simple process, high yield and the like.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing N,N-diethylisopropylamine. Background technique [0002] N,N–Diethylisopropylamine (N,N-Diethylisopropylamine), which has the molecular formula C 7 h 17 N, whose structural formula is shown in S-1, has a boiling point of 107.5~108.0°C. It has a wide range of industrial applications and is an important fine chemical raw material. It is also an important pharmaceutical, pesticide intermediate, and quaternary ammonium compound intermediate. Manufacture of pharmaceutical anesthetics, pesticides and herbicides, etc. [0003] [0004] S-1 [0005] [0006] S-2 [0007] [0008] S-3 [0009] [0010] S-4 [0011] [0012] S-5 [0013] Based on literature reports, at present the preparation of N,N,-diethylisopropylamine adopts the following methods: 1, using nickel as a catalyst, adopting triethylsilane and N-ethoxymethyldiisop...

Claims

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Application Information

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IPC IPC(8): C07C211/08C07C209/74
Inventor 陈新志罗虎钱超
Owner ZHEJIANG UNIV
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