反应详情

温度

80 °C

To a stirred solution of 1-bromo-2-(bromomethyl)-4-chlorobenzene (1.70 g, 6 mmol) in ACN (10.0 mL) was added p-methoxybenzyl amine (0.91 g, 6.6 mmol) and potassium carbonate (2.08 g, 15.0 mmol) and the overall mixture was stirred at 80° C. overnight. After cooling, the reaction mixture was diluted with water (10 mL) and diluted with EtOAc (15 mL). The separated aqueous layer was extracted with EtOAc (10 mL×2) and the combined organic layers were washed with brine, dried over Na2SO4, and concentrated to give a crude residue which was washed with hexanes to obtain the desired product N-(4-methoxybenzyl)(2-bromo-5-chlorophenyl)methanamine as a pale yellow solid. MS m/e 340 (M+H)+.

1. temperatureAfter cooling
2. extractionThe separated aqueous layer was extracted with EtOAc (10 mL×2)
3. washthe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto give a crude residue which
7. washwas washed with hexanes