反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
4-Bromo-1-(4-trifluoromethoxyphenyl)-1H-imidazole (100 mg, 0.326 mmol), 2-formyl-5-methoxyphenylboronic acid (73 mg, 0.41 mmol), bis(triphenylphosphine)palladium dichloride (2 mg, 0.003 mmol), NaHCO3 (49 mg, 0.59 mmol) and 1:1 DME/H2O (8:8 mL) were combined and added to a microwave vessel. The reaction mixture was heated in the microwave with stirring at 100° C. for 12 min. The microwave took 5 min to reach 100° C., then maintained at 100° C. for 12 min, and then cooled. TLC (1:1 EtOAc:cyclohexane) showed the presence of starting materials, thus the sample was heated to 100° C. for another 8 min. Upon cooling a precipitate formed; this was filtered and washed with H2O to give a grey solid (86 mg): ESIMS m/z 363.0 (M+H).
WORKUP
后处理
- additionadded to a microwave vessel
- temperatureThe reaction mixture was heated in the microwave
- waitThe microwave took 5 min
- customto reach 100° C.
- temperaturemaintained at 100° C. for 12 min
- temperaturecooled
- temperaturethus the sample was heated to 100° C. for another 8 min
- temperatureUpon cooling a precipitate
- customformed
- filtrationthis was filtered
- washwashed with H2O