2-(5-溴-2-氟苯基)乙酰基 氯化物

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

实验步骤: To a mixture of allyl alcohol (22.1 g, 380.5 mmol) and triethylamine (Et3N) (5.4 ml, 39 mmol) at 0° C. was added over 1 h crude (5-bromo-2-fluoro-phenyl) -acetyl chloride (intermediate B2A) (7.01 g, ca. 26 mmol). Then the reaction was stirred over 1 h from 0° C. to 23° C. The reaction mixture was diluted with ethyl acetate, washed with water, and the organic layer was dried over sodium sulfate. Removal of the solvent in vacuum left the title compound as a yellow oil (7.290 g, 103%), which was used without further purification. MS (ISP): m/z=280.1 [(M+NH4)+] and 282.1 [(M+2+NH4)+] washed with water the organic layer was dried over sodium sulfate Removal of the solvent in vacuum left the title compound as a yellow oil (7.290 g, 103%), which was used without further purification

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a mixture of commercially available 5-bromo-2-fluorophenylacetic acid (compound B1A, [CAS No. 883514-21-4], 6.42 g, 26 mmol) in toluene (52 ml) and thionyl chloride (SOCl2) (4.721 ml, 40 mmol) at 23° C. was added a drop of N,N-dimethylformamide (DMF) and the mixture was stirred at 80° C. for 4 hours (reaction checked by HPLC with product+MeOH). All volatiles were removed by rotary evaporation and the residue was dried in high vacuum to give the title compound as a colorless liquid (7.01 g, 105%), which was used without further purification. All volatiles were removed by rotary evaporation the residue was dried in high vacuum