Application of 67442-07-3, A common heterocyclic compound, 67442-07-3, name is 2-Chloro-N-methoxy-N-methylacetamide, molecular formula is C4H8ClNO2, 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.
Under nitrogen protection, 1340.5g of intermediate was taken, dissolved in 200mL anhydrous THF, the reaction system was cooled to -15¡ã, and 13g of THF solution of 13g isopropylmagnesium chloride was added dropwise. During the dropwise addition, the reaction temperature was controlled at -5¡ã. After the completion of the dropwise addition, the reaction was continued for 1 h, and then 60 g of a solution of 15 g of 2-chloro-N-methoxy-N-methylacetamide in THF was added dropwise thereto, and the reaction temperature was controlled not to exceed -5¡ã during the dropwise addition. After the end of the addition, the temperature of the system was raised to -5-0 ¡ã, and after the reaction was completed, the reaction was quenched by the addition of 2N hydrochloric acid at 0 ¡ã, and ethyl acetate (200 mL) was added, and the mixture was separated. , filtration, solvent recovery under reduced pressure, residue,With methanol:Water = 10:1 recrystallized to give a white solid, 27 g, yield 76percent.
The synthetic route of 67442-07-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Jiangsu Engineering Polytechnic College; Feng Chengliang; Yao Wenjin; Yan Bin; (12 pag.)CN109678686; (2019); A;,
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