反应 #2088689
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06500840B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 2-amino-1-(3-chlorophenyl)ethanone hydrochloride from Step 79a (2.83 g, 13.7 mmol, 1 eq), ethyl chlorooxoacetate (1.87 g, 13.7 mmol, 1 eq), and CH2Cl2 (40 mL) is cooled in an ice-H2O bath. The mixture is treated with a solution of TEA (4.0 mL, 29 mmol, 2.1 eq) in CH2Cl2 (20 mL), and the reaction is warmed to room temperature overnight. Water is added and the organic layer is separated, dried over MgSO4, filtered., and evaporated. The resulting solid is triturated with hexane/2-propanol and dried in vacuo to provide the title compound (2.70 g, 72%). MS (ESI) for C12H12ClNO4 m/z 270 (M+H)+. is cooled in an ice-H2O bath the organic layer is separated dried over MgSO4 filtered , and evaporated The resulting solid is triturated with hexane/2-propanol dried in vacuo
来源 ID: ord-d2b51a6f48944de1923abf378cf4311c