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Method for synthesizing 2-methyl-1,2-propane diamine

A synthesis method, the technology of propylenediamine, applied in the field of catalytic synthesis, can solve the problems of complex synthesis steps, unstable raw materials, and long time consumption, and achieve the effects of clean synthesis process, lower production cost, and simple operation

Active Publication Date: 2014-03-12
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a clean and easy-to-industrialize synthetic method of 2-methyl-1,2-propanediamine aiming at the shortcomings of existing methods such as unstable raw materials, complex synthesis steps, and long time consumption

Method used

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  • Method for synthesizing 2-methyl-1,2-propane diamine
  • Method for synthesizing 2-methyl-1,2-propane diamine

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Experimental program
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Effect test

Embodiment 1

[0027] Add 110g of 2-amino-2-methyl-1-propanol and 3.3g of Raney Ni catalyst into the autoclave, replace the air in the autoclave with hydrogen, then pump the vacuum, feed 42g of liquid ammonia, and continue to feed hydrogen to 2MPa , heated up to 185°C, and reacted for 8h. After the reaction, the reaction solution was cooled to room temperature, and the reaction solution was filtered to recover the catalyst. Based on the consumption of 2-amino-2-methyl-1-propanol per unit weight, the conversion rate is 55.2%, and the selectivity of 2-methyl-1,2-propanediamine is 81.0%.

Embodiment 2

[0029] Add 95g of 2-amino-2-methyl-1-propanol and 2.9g of Raney Ni catalyst into the autoclave, replace the air in the autoclave with hydrogen, then pump the vacuum, feed 45g of liquid ammonia, and continue to feed hydrogen to 3MPa , heated up to 195°C, and reacted for 8h. After the reaction, the reaction solution was cooled to room temperature, and the reaction solution was filtered to recover the catalyst. Based on the consumption of 2-amino-2-methyl-1-propanol per unit weight, the conversion rate is 59.5%, and the selectivity of 2-methyl-1,2-propanediamine is 85.6%.

Embodiment 3

[0031] Add 95g of 2-amino-2-methyl-1-propanol and 4.8g of Raney Ni catalyst into the autoclave, replace the air in the autoclave with hydrogen, then pump the vacuum, feed 45g of liquid ammonia, and continue to feed hydrogen to 3MPa , heated up to 185°C, and reacted for 12h. After the reaction, the reaction solution was cooled to room temperature, and the reaction solution was filtered to recover the catalyst. Based on the consumption of 2-amino-2-methyl-1-propanol per unit weight, the conversion rate is 63.5%, and the selectivity of 2-methyl-1,2-propanediamine is 83.8%.

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Abstract

The invention relates to a method for synthesizing 2-methyl-1,2-propane diamine. According to the method, 2-amino-2-methyl-1-propanol taken as a raw material is subjected to catalytic amination to generate 2-methyl-1,2-propane diamine under hydrogen condition. The method comprises the following steps: (1) adding 2-amino-2-methyl-1-propanol and a catalyst into a high-pressure autoclave; (2) replacing air in the autoclave with hydrogen and then vacuumizing; (3) introducing liquid ammonia and hydrogen, and reacting at 160-220 DEG C; and (4) filtering to remove the catalyst after the reaction is ended, and rectifying reaction solution to obtain the purified 2-methyl-1,2-propane diamine. The process has the advantages that the performances of the raw material are stable, the synthesis steps are simple and the yield is high; moreover, the whole process can be carried out continuously, so that the production cost is further reduced.

Description

technical field [0001] The invention belongs to the field of catalytic synthesis, and in particular relates to a synthesis method of 2-methyl-1,2-propanediamine. Background technique [0002] 2-Methyl-1,2-propanediamine is an important intermediate for the preparation of a new generation of antimalarial drug OZ277 (Arterolane). OZ277 overcomes the resistance of pathogens to traditional antimalarial drugs, and is effective when taken orally, has low toxicity, is easy to absorb, has a long duration of drug effect, and has a broad market prospect. The corresponding intermediate 2-methyl-1,2-propanediamine The demand is also increasing year by year. In addition, 2-methyl-1,2-propanediamine is also an ideal raw material for preparing batteries, metal chelating agents, polyamides, etc. [0003] At present, there are few reports on the synthesis methods of 2-methyl-1,2-propanediamine at home and abroad. Chinese patent CN102976951A reports a preparation method of 2-methyl-1,2-pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/11C07C209/16
Inventor 王为强吕剑余秦伟杨建明梅苏宁王伟李亚妮赵锋伟张前万洪
Owner XIAN MODERN CHEM RES INST