反应详情

Under an argon stream, zinc powder (11 g, 267 mmol) was suspended in tetrahydrofuran (30 ml), 1,2-dibromoethane (0.15 ml, 1.8 mmol) and trimethylsilyl chloride (0.45 ml, 3.6 mmol) were added at 65° C., and the mixture was stirred with heating for 30 min. A solution of 3-chloro-2-fluorobenzyl bromide (41 g, 178 mmol) in tetrahydrofuran (100 ml) was added dropwise at 65° C., and the mixture was stirred with heating for 2 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 2 hr