Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 67442-07-3, name is 2-Chloro-N-methoxy-N-methylacetamide, A new synthetic method of this compound is introduced below., Computed Properties of C4H8ClNO2
A solution of 2.5 M n-butyl lithium in hexanes (35ml, 87.6mmol) was added to a solution of the bromide from preparation 29 (20.0g, 79.7mmol) in ferf-butyl methylether (300ml) at -78¡ãC under nitrogen over 10 minutes. The reaction was stirred for a further 10 minutes and 2-chloro-N-methoxy-N-methyl-acetamide (12.1g, 87.6mmol) in terf-butyl-methylether (40ml) was added slowly. The reaction was stirred at -78¡ãC for 20 minutes and then 1M hydrochloric acid (200ml) was added. The mixture was allowed to warm to room temperature, stirred for 2 hours and the organic phase separated. The aqueous phase was extracted with fe/f-butyl methylether and the combined organic extracts were washed with water (100ml), saturated aqueous sodium chloride (100ml) and 1M sodium hydroxide (100ml). The organic phase was dried (sodium sulfate), concentrated in vacua and the residual oil purified by flash column chromatography on silica gel eluting with pentane:dichloromethane:methanol (75:25:0 changing to 0:99:1, by volume). The residue was recrystallised from pentane:dichloromethane to give the title compound as a yellow solid.1H NMR (400MHz, CDCI3): 5 = 9.11 (1H, s), 8.34-8.33 (1H, d), 7.32-7.30 (1H,d), 5.91 (2H, s), 4.66 (2H, s), 2.17 (6H, s) ppm.LRMS (electrospray): m/z [M-H]+ 247.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2004/108676; (2004); A1;,
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