1-(溴甲基)-4-乙炔苯

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

实验步骤: 4-Ethynylbenzyl alcohol a (1 g, 7.57 mmol) was diluted in 20 ml DCM, and cooled to 0° in ice bath. Phosphorus tribromide (4.1 g, 15 mmol) was added dropwise. The reaction was allowed to warm to room temperature gradually, and stirred under nitrogen overnight. The reaction was quenched by addition of H2O in ice bath, extracted by DCM. Combined organic layers were washed with brine, dried over Na2SO4 and concentrated to dryness. The crude material was purified by chromatography (ISCO) using 100% hexane to give pure 4-ethynylbenzyl bromide b (220 mg). M+H+ 195.1 cooled to 0° in ice bath The reaction was quenched by addition of H2O in ice bath extracted by DCM Combined organic layers were washed with brine dried over Na2SO4 concentrated to dryness The crude material was purified by chromatography (ISCO)