3'-溴-2'-氯苯乙酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 3-bromo-2-chloro-N-methoxy-N-methylbenzamide (0.71 mmol) in 7 mL THF was added a solution of MeMgBr (4.31 mmol, 3M solution in Et2O) at 0° C. The cooling bath was removed after 1 h and stirring was continued at RT overnight. The reaction was quenched with water and sat. aq. NH4Cl solution under cooling. The mixture was extracted with EtOAc (3×), the combined organic layers were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification by CC (KP-SIL™ from Biotage) using Hept to Hept/EtOAc (85/15) gives the desired compound as colorless oil; The cooling bath was removed after 1 h The reaction was quenched with water and sat. aq. NH4Cl solution under cooling The mixture was extracted with EtOAc (3×) the combined organic layers were washed with brine dried over MgSO4 concentrated in vacuo Purification by CC (KP-SIL™ from Biotage)