反应详情

温度

110 °C

A 100 mL round bottom flask was mixed with 4-triflouromethylbromobenzene (3.2 g, 15.0 mmol), triisopropylphosphine (10.0 mg, 0.062 mmol), Pd(OAc)2 (3.0 mg, 0.013 mmol) and xylenes (50 mL). The reaction mixture was allowed to heat at 110° C. for a period of 30 min at which it was mixed with tert-butyl piperidin-4-ylcarbamate (1.0 g 5.0 mmol). The reaction mixture stirred at 120° C. for 4.0 hours and then cooled to RT. The reaction mixture was partitioned between EtOAc and saturated NaHCO3. The organics were dried over MgSO4 and concentrated to a crude oil. The oil was purified using silica gel chromatography (90% hexanes/10% EtOAc) to yield a total of 472 mg of mostly pure solid.

1. temperaturecooled to RT
2. customThe reaction mixture was partitioned between EtOAc and saturated NaHCO3
3. dry with materialThe organics were dried over MgSO4
4. concentrationconcentrated to a crude oil
5. customThe oil was purified
6. customto yield a total of 472 mg of mostly pure solid