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Green and environment-friendly synthesis method of N, N, N'-trimethylethylenediamine

A technology of trimethylethylenediamine and its synthesis method, which is applied in the preparation of amino-substituted functional groups, organic chemistry, etc., and can solve problems such as difficult handling and high salt

Active Publication Date: 2019-12-13
XIAN RUILIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this process is the safety risk when adding solid alkali for alkalization
At the same time, this process also produces a large amount of high-salt, high-ammonia nitrogen wastewater, which is difficult to treat

Method used

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  • Green and environment-friendly synthesis method of N, N, N'-trimethylethylenediamine
  • Green and environment-friendly synthesis method of N, N, N'-trimethylethylenediamine
  • Green and environment-friendly synthesis method of N, N, N'-trimethylethylenediamine

Examples

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Embodiment 1

[0039] A green and environment-friendly synthesis method of N,N,N'-trimethylethylenediamine, the specific preparation process flow chart is as follows figure 1 shown, including the following steps:

[0040] S1, Preparation of N,N,N'-trimethylethylenediamine hydrochloride

[0041] Add 311.5 g of a 40% dimethylamine aqueous solution in a closed three-necked flask with a mechanical stirrer and a thermometer, and add 600 g of 50% 2-chloro-N- The solution of methylethylamine hydrochloride was reacted, and the reaction solution was obtained after 2 hours of reaction;

[0042] S2, post-processing

[0043] The three-necked flask in S1 is connected in series with the dimethylamine absorption device with an air guide tube, and 3500 g of mass concentration is 25% hydrochloric acid solution is housed in the dimethylamine absorption device, and 576.9 g of 64% hydrochloric acid solution is added dropwise to the three-necked flask under stirring conditions. Sodium hydroxide aqueous soluti...

Embodiment 3

[0055] A green and environment-friendly synthetic method of N,N,N'-trimethylethylenediamine, comprising the steps of:

[0056] S1, Preparation of N,N,N'-trimethylethylenediamine hydrochloride

[0057] Add 1617.2 g of a 40% methylamine aqueous solution with a mass concentration of 40% in a closed three-necked flask with a mechanical stirrer and a thermometer, and add 750 g of 40% N, N-dimethylamine dropwise at 40° C. Aminochloroethane hydrochloride aqueous solution was reacted, and after the dropwise addition was completed, it was reacted for 6 hours to obtain a reaction solution;

[0058] S2, post-processing

[0059] Connect the methylamine absorption device on the three-necked flask with an air guide tube. The methylamine absorption device is equipped with 4000g of mass concentration and is 20% hydrochloric acid solution. Under stirring conditions, add 238.0g of mass concentration to the three-necked flask dropwise. 70% sodium hydroxide aqueous solution , and the temperatur...

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Abstract

The invention discloses a green and environment-friendly synthesis method of N, N, N'-trimethylethylenediamine. The preparation method comprises the following steps: adding an aqueous solution of methylamine or dimethylamine into a reaction container, dropwise adding an aqueous solution of N, N-dimethylaminochloroethane hydrochloride into the methylamine when the methylamine is added into the reaction container, dropwise adding an aqueous solution of 2-chloro-N-methylethylamine hydrochloride into the dimethylamine when the dimethylamine is added into the reaction container, and obtaining a reaction solution after the reaction is finished; connecting the reaction container with a methylamine absorption device in series, dropwise adding an inorganic alkali solution into the reaction solution, and respectively collecting an organic phase and an alkaline water phase; rectifying the organic phase to obtain a product; concentrating the alkaline water phase until the amount of the concentrated water is the sum of the water content of raw materials, filtering, and recovering alkaline liquid. According to the method, the methylamine or a substituted methylamine gas is absorbed by a dilute acid, so that the safety risk caused by escape of a large amount of the methylamine or substituted methylamine is avoided, zero emission of wastewater and solid waste is realized, and the recycling rate tends to 100%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and specifically discloses a green and environment-friendly synthesis method of N,N,N'-trimethylethylenediamine. Background technique [0002] Ethylenediamine derivatives are synthetic raw materials and intermediates of many fine chemical products such as medicines, materials, and additives, and are widely used in the synthesis of kinase inhibitors, surfactants, and fungicides. In recent years, N,N,N'-trimethylethylenediamine has been used as the main intermediate of various kinase inhibitors, such as osimertinib for the treatment of advanced lung cancer, a compound with JAK kinase inhibitory activity, and its market The demand is increasing, and as a pharmaceutical intermediate, there are also higher requirements for its purity and production process. It is of great significance to study its green preparation method suitable for large-scale industrial production. [0003] CN201310415...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/08C07C211/10
CPCC07C209/08C07C211/10
Inventor 高仁孝段迎春冯小琼杨军义曹晓峰王磊
Owner XIAN RUILIAN NEW MATERIAL CO LTD
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