反应详情

To a stirred mixture of Zn metal (18.5 g, 289.06 mmol, 1.09 equiv), I2 (500 mg, 1.97 mmol, 0.01 equiv) and 1-(bromomethyl)-4-fluorobenzene (5 g, 0.10 equiv) in anhydrous tetrahydrofuran (50 mL) maintained under nitrogen at room temperature was added dropwise a solution of 1-(bromomethyl)-4-fluorobenzene (45 g, 211.6 mmol, 0.90 equiv) in tetrahydrofuran (200 mL). TMSCl (500 mg, 4.60 mmol, 0.02 equiv) was then added dropwise to the reaction. The resulting mixture was refluxed for 10 h. The solution was cooled to 0° C. and used in the next step immediately.

1. temperatureThe resulting mixture was refluxed for 10 h
2. temperatureThe solution was cooled to 0° C.