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Synthesizing method of N,N-diisopropyl butylamine

A technology of propylbutylamine and synthesis method, which is applied in the field of N, can solve the problems of expensive raw materials, perishable, and many by-products, and achieve the effects of easy-to-obtain raw materials, low production costs, and easy industrialization

Inactive Publication Date: 2010-02-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main shortcoming of this method is that raw material is expensive, perishable, and by product is many, and its yield is (yield is 50%)

Method used

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  • Synthesizing method of N,N-diisopropyl butylamine
  • Synthesizing method of N,N-diisopropyl butylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Embodiment 1, a kind of synthetic method of N, N-diisopropylbutylamine:

[0013] Add 84ml (0.6mol) of diisopropylamine and 32ml (0.3mol) of 1-chlorobutane into an autoclave with a stirring temperature measuring device, and close the lid of the kettle. The temperature was raised to 200°C within 1h, and the pressure was 1.36Mpa at this time. After maintaining the temperature and pressure for 4 hours, the reaction was terminated.

[0014] NaOH solution was added to the obtained reaction solution until the pH=13, the organic phase was separated and rectified, and the fraction at 162-163°C was collected to obtain 31.9 g of N,N-diisopropylbutylamine with a yield of 67.59%.

Embodiment 2

[0015] Embodiment 2, a kind of synthetic method of N, N-diisopropylbutylamine:

[0016] Add 127ml (0.9mol) of diisopropylamine and 32ml (0.3mol) of 1-chlorobutane into an autoclave with a stirring temperature measuring device, and close the lid of the kettle. The temperature was raised to 200°C within 1h, and the pressure was 1.36Mpa at this time. After maintaining the temperature and pressure for 4 hours, the reaction was terminated.

[0017] NaOH solution was added to the obtained reaction liquid until PH=13, the organic phase was separated and rectified, and the fraction at 162-163°C was collected to obtain 32.2 g of N,N-diisopropylbutylamine with a yield of 68.23%.

Embodiment 3

[0018] Embodiment 3, a kind of synthetic method of N, N-diisopropylbutylamine:

[0019] Add 127ml (0.9mol) of diisopropylamine and 32ml (0.3mol) of 1-chlorobutane into an autoclave with a stirring temperature measuring device, and close the lid of the kettle. The temperature was raised to 200°C within 1h, and the pressure was 1.36Mpa at this time. After maintaining the temperature and pressure for 8 hours, the reaction was terminated.

[0020] NaOH solution was added to the obtained reaction liquid until PH=13, the organic phase was separated and rectified, and the fraction at 162-163°C was collected to obtain 39.7 g of N,N-diisopropylbutylamine with a yield of 84.13%.

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Abstract

The invention discloses a synthesizing method of N,N-diisopropyl butylamine, which comprises the following steps: using diisopropylamine and 1-chlorobutane as raw materials to carry out a reaction in a high-pressure kettle under reaction pressure of 1.05-2.0Mpa and a reaction temperature of 150-250 DEG C for 4-10 hours in a molar ratio of the diisopropylamine to the 1-chlorobutane of 2-5:1; regulating the pH of the resulting reaction solution to be 12.5-13.5; and then separating out an organic phase to rectify so as to obtain the N,N-diisopropyl butylamine. The N,N-diisopropyl butylamine synthesized by the method has the characteristics of low production cost, 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-diisopropylbutylamine. Background technique [0002] N,N-Diisopropylbutylamine is a weakly basic tertiary amine, a chemical intermediate used in organic synthesis, and its structural formula is as follows: [0003] [0004] N, the synthetic method of N-diisopropylbutylamine is less seen in the report, mainly adopts organolithium reagent reaction to obtain, as document (Synthesis, 1997,545-548) report adopts The reaction yields the target product. The main shortcoming of this method is that raw material is expensive, perishable, and by-product is many, and its yield is (yield is 50%). Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a synthetic method of N,N-diisopropylbutylamine with low cost and high yield. [0006] In order to solve the above-mentioned technical probl...

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
Owner ZHEJIANG UNIV
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