Application of 100-37-8 ,Some common heterocyclic compound, 100-37-8, molecular formula is C6H15NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
Add 146g of thionyl chloride and 240g of dichloromethane to the 1L reaction bottle to cool down, use 500ml beaker during cooling processA mixed solution of 120 g of diethylaminoethanol and 100 g of dichloromethane was prepared. When the temperature in the reaction flask was lowered to -10 C, a mixture of diethylaminoethanol and dichloromethane was added dropwise at a temperature of -10 to 20 C. 1 hour and 28 minutes, the addition is completed;After the completion of the dropwise addition, the temperature was raised to 20 to 45 C for 5 hours, and after the completion of the incubation, the dichloromethane was concentrated for 1 hour and 05 minutes.Concentrated to a total of 258g of dichloromethane, the recovery of dichloromethane can be directly applied;After concentration and drying, the temperature was lowered to 27 C. 240 g of absolute ethanol was added to the reaction flask and heated to dissolve the solid.After dissolving, the ice brine was cooled to -5 to -10 C for 6 hours, and filtered to obtain 2-diethylaminochloroethane hydrochloride wet product 177.6 g wet.Product.After the mother liquor is collected, 208g of ethanol is concentrated and recovered. The recovered ethanol can be continuously applied, and the residual liquid is placed in a freezer for freezing and crystallization. After hourly filtration, 18.5 g of the mother liquor product was obtained, and then recrystallized from 32 g of recovered ethanol to obtain 13.8 g of a qualified mother liquor. A total of 191.4 g of the combined product was dried at 55-60 C to obtain 173.9 g of dry product of 2-(diethylamino)ethyl chloride hydrochloride, and the liquid phase purity was 99.82%, and the molar yield was calculated to be 98.7%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,100-37-8, its application will become more common.
Reference:
Patent; Shandong Cheng Hui Shuang Da Pharmaceutical Co., Ltd.; Wang Yongguang; Liu Xuewen; Xue Qimeng; Zhao Zhonggui; Xu Linjie; (9 pag.)CN108084033; (2018); A;,
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