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Synthesis method of N, N, N', N'-tetraisopropyl ethylene diamine

A technique of propylethylenediamine and its synthesis method, which is applied in the field of N, can solve problems such as the difficulty of solvent recovery and mechanical application, increase the difficulty of product separation, and the high price of dibromoethane, and achieve low price, reduced pressure, and simple post-treatment Effect

Active Publication Date: 2010-12-29
CHINA CONSTR IND & ENERGY ENG GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses ethanol as a solvent, which increases the difficulty of product separation and the difficulty of solvent recovery and mechanical application. At the same time, the price of raw material dibromoethane is high, the yield is low, and the pollution is serious.

Method used

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  • Synthesis method of N, N, N', N'-tetraisopropyl ethylene diamine
  • Synthesis method of N, N, N', N'-tetraisopropyl ethylene diamine
  • Synthesis method of N, N, N', N'-tetraisopropyl ethylene diamine

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Example 1. A method for synthesizing N,N,N',N'-tetraisopropylethylenediamine:

[0019] Add 40.5 g (0.4 mol) of diisopropylamine and 39.6 g (0.4 mol) of dichloroethane into the autoclave with a stirring temperature measuring device, and close the lid. Use N 2 After detecting 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 keeping the temperature for 4 hours.

[0020] Add NaOH aqueous solution (mass concentration 50%) to the obtained solid-liquid mixture until PH=13.5, stand still for layering, separate the organic phase (located in the upper layer) and perform intermittent distillation under reduced pressure (1266.6Pa), collect 86.5-97.0℃ From the distillate, 38.9 g of N,N,N′,N′-tetraisopropylethylenediamine was obtained, the yield was 85.2%, and the purity was 99%. The obtained product was characterized by a correct structure.

Embodiment 2

[0021] Example 2. A method for synthesizing N,N,N',N'-tetraisopropylethylenediamine:

[0022] Add 40.5g (0.4mol) of diisopropylamine and 79.2g (0.8mol) of dichloroethane into the autoclave with a stirring temperature measuring device, and close the lid of the kettle. Use N 2 After detecting 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 keeping the temperature for 6 hours.

[0023] Add KOH aqueous solution (mass concentration 50%) to the obtained solid-liquid mixture until PH=13.5, stand still for stratification, separate the organic phase (located in the upper layer) and perform intermittent distillation under reduced pressure (1266.6Pa), collect 86.5-97.0℃ From the distillate, 40.3 g of N,N,N',N'-tetraisopropylethylenediamine was obtained, the yield was 88.2%, and the purity was 99%. The resulting product was characterized by a correct structure.

Embodiment 3

[0024] Example 3. A method for synthesizing N,N,N',N'-tetraisopropylethylenediamine:

[0025] Add 40.5g (0.4mol) of diisopropylamine and 79.2g (0.8mol) of dichloroethane into the autoclave with a stirring temperature measuring device, and close the lid of the kettle. Use N 2 After detecting leaks and replacing the air several times, the temperature was raised to 140°C and the pressure was 0.5MPa. The reaction was terminated after keeping the temperature for 8 hours.

[0026] Add Na to the resulting solid-liquid mixture 2 CO 3 Aqueous solution (mass concentration 20%) until PH=11.5, stand still for stratification, separate the organic phase (located in the upper layer) and perform intermittent distillation under reduced pressure (1266.6Pa), collect fractions at 86.5-97.0°C to obtain products N, N, N ',N'-tetraisopropylethylenediamine 40.2g, the yield was 88.0%, the purity was 99%, and the resulting product was characterized by the correct structure.

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Abstract

The invention discloses a synthesis method of N, N, N', N'-teraisopropyl ethylene diamine. Diisopropylamine and dichloroethane are taken as raw materials, reaction is carried out in a high pressure autoclave under the conditions of no solvent and no catalyst, the mol ratio of diisopropylamine and [to] dichloroethane is 1: 1-4, reaction temperature is 100-200 DEG C, reaction pressure is 0.2-1.1Mpa, reaction time is 4-10 hours, so as to obtain solid liquid mixture; alkaline aqueous solution is added into the solid liquid mixture until pH value is 11.5-13.5; and finally separation and reduced pressure rectification are carried out, thus obtaining N, N, N', N'-teraisopropyl ethylene diamine. The method for synthesizing N, N, N', N'-teraisopropyl ethylene diamine of the invention has the characteristics of simple process and high yield and is environmentally friendly.

Description

Technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing N,N,N',N'-tetraisopropylethylenediamine. Background technique [0002] N,N,N′,N′-Tetraisopropylethylenediamine (N,N,N′,N′-Tetraisopropylethylenediamine), its molecular formula is C 14 H 32 N 2 Its structural formula is as shown in S-1, and its boiling point is 237.3~238.2℃. It has a wide range of industrial uses and is an important fine chemical raw material. It can be used not only as a biochemical reagent, epoxy resin crosslinking agent, but also as a quaternary amine Compound intermediates. [0003] [0004] [0005] [0006] [0007] According to comprehensive literature reports, the current preparation of N,N,N',N'-tetraisopropylethylenediamine adopts the following methods: 1. Diacetyl chloride is reacted with diisopropylamine to generate amide, which is then reduced by lithium aluminum hydride. N,N,N',N'-tetraisopropylethylenediamine is obta...

Claims

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Application Information

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IPC IPC(8): C07C211/10C07C209/08
Inventor 陈新志罗虎钱超
Owner CHINA CONSTR IND & ENERGY ENG GRP CO LTD
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