反应详情

Under an argon stream, zinc powder (11 g, 175 mmol) was suspended in tetrahydrofuran (30 ml), 1,2-dibromoethane (0.1 ml, 1.20 mmol) and trimethylsilyl chloride (0.29 ml, 2.4 mmol) were added at 60° C., and the mixture was stirred with heating for 30 min. A solution of 3-chloro-2-fluorobenzyl bromide (27 g, 119 mmol) in tetrahydrofuran (60 ml) was added dropwise at 60° C. The mixture was stirred with heating for 1 hr and allowed to cool to room temperature to give a solution of 1M 3-chloro-2-fluorobenzylzinc bromide in tetrahydrofuran. This was used in the next main step.

1. temperaturewith heating for 30 min
2. stirringThe mixture was stirred
3. temperaturewith heating for 1 hr