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A green and environment-friendly synthetic method of n,n,n'-trimethylethylenediamine
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A technology of trimethylethylenediamine and a synthesis method, which can be applied in the preparation of amino-substituted functional groups, organic chemistry, etc., and can solve the problems of high salt and difficult handling.
Active Publication Date: 2022-06-24
XIAN RUILIAN NEW MATERIAL CO LTD
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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
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Embodiment 1
[0039] A kind of green and environment-friendly synthetic method of N,N,N'-trimethylethylenediamine, the specific preparation process flow chart is as follows figure 1 shown, including the following steps:
[0040] Preparation of S1,N,N,N'-trimethylethylenediamine hydrochloride
[0041] To a closed three-necked flask with mechanical stirring and a thermometer, add 311.5 g of a 40% dimethylamine aqueous solution with a mass concentration, and at 0° C., dropwise add 600 g of 50% 2-chloro-N- The solution of methylethylamine hydrochloride is reacted, and the reaction solution is obtained after the reaction for 2h;
[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. The dimethylamine absorption device is equipped with 3500g of hydrochloric acid solution with a mass concentration of 25%. Sodium hydroxide aqueous solution, and the temperature of sodium hydroxide aqueous solution ...
Embodiment 3
[0055] A green and environment-friendly synthetic method of N,N,N'-trimethylethylenediamine, comprising the following steps:
[0056] Preparation of S1,N,N,N'-trimethylethylenediamine hydrochloride
[0057] To the closed three-necked flask with mechanical stirring and thermometer, add 1617.2 g of methylamine aqueous solution with a mass concentration of 40%, and at 40° C., dropwise add 750 g of N,N-dimethylamine with a concentration of 40% to the methylamine aqueous solution The aqueous solution of aminochloroethane hydrochloride is reacted, and the reaction is performed for 6 hours after the dropwise addition to obtain a reaction solution;
[0058] S2, post-processing
[0059] A methylamine absorption device was connected to the three-necked flask with an air guide, and 4000 g of a 20% hydrochloric acid solution was installed in the methylamine absorption device, and 238.0 g of an aqueous sodium hydroxide solution with a mass concentration of 70% was added dropwise to the th...
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Abstract
The invention discloses a green and environment-friendly synthesis method of N,N,N'-trimethylethylenediamine, which comprises the following steps: adding an aqueous solution of methylamine or dimethylamine into a reaction vessel, and adding formazan to the reaction vessel For amine, add N, N-dimethylaminochloroethane hydrochloride solution dropwise to methylamine, when adding dimethylamine to the reaction vessel, add 2-chloro-N-methylethyl ether dropwise to dimethylamine Amine hydrochloride aqueous solution, the reaction solution is obtained after the reaction is completed; the reaction vessel is connected in series with the methylamine absorption device, and the inorganic alkali solution is added dropwise to the reaction solution, and the organic phase and the alkali aqueous phase are collected respectively; the product is obtained after the organic phase is rectified; the alkali The water phase is concentrated until the concentrated water is equal to the sum of the water contained in the raw materials, and then filtered to recover the lye. The invention absorbs methylamine or substituted methylamine gas through dilute acid, which solves the safety risk caused by the escape of a large amount of methylamine or substituted methylamine. The invention also realizes zero discharge of waste water and solid waste, and the recovery rate is applied mechanically. Tend 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 the synthetic raw materials and intermediates of many fine chemical products such as medicines, materials and auxiliaries. They 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, compounds 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 industrialized large-scale production. [0003] CN...
Claims
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