In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine, the common compound, a new synthetic route is introduced below. name: N-((6-Chloropyridin-3-yl)methyl)ethanamine
General procedure: This embodiment is basically the same as Embodiment 1, except that:Step 2, using 170 g (15%) sodium carbonate instead of 52 g (40%) potassium carbonate aqueous solution, 41.8 g (98%) 2-chloro-5-ethylaminomethylpyridine instead of 40% methylamine.As a result, 70.5 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N’-(6-chloro-3-pyridylmethyl)-N’-ethyl-2- Nitrovinylidene diamine, content 98.1%, yield 83.1%. _: 2 In a 500 mL four-necked flask, 35.1 g (89%) of 1,1-dichloronitroethylene (0.22 mol) and 150 mL of dichloromethane were added.Stirring was carried out to 0 to 10 C, and 36.2 g (98%) of 2-chloro-5-ethylaminomethylthiazole (0.2 mol) was added dropwise. After the addition, 52 g (40%) of potassium carbonate aqueous solution was added dropwise at this temperature. , keep warm for 2 hours,Sampling HPLC analysis of N-(2-chloro-5-thiazole) methyl-N-ethylamine conversion rate of 98% or more, adding 38.8g (40%) methylamine aqueous solution (0.5mol) at 5-10 C, plus Stir for 1 hour after finishing.The temperature was raised to 20 to 25 C for 2 hours, and the oil layer was separated and allowed to stand, and the aqueous layer was extracted with dichloromethane for 3 times.The oil layer was desolvated, and 70 g of ethyl acetate was added to the residue, stirred well, and cooled to 0 to 5 C for filtration.Drying to obtain 50 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N’-methyl-2-nitrovinylidene diamine, content 98%, yield 88.6% .
The synthetic route of 120739-77-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Lianyungang Liben Crop Technology Co., Ltd.; Wu Hailin; Dong Junjie; Dai Zhanyong; Gong Jian; Li Datie; (6 pag.)CN107474022; (2017); A;,
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