HRID708946

反应详情

EQUATION

反应方程式

HRID 708946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. additionadded to a microwave vessel
  2. temperatureThe reaction mixture was heated in the microwave
  3. waitThe microwave took 5 min
  4. customto reach 100° C.
  5. temperaturemaintained at 100° C. for 12 min
  6. temperaturecooled
  7. temperaturethus the sample was heated to 100° C. for another 8 min
  8. temperatureUpon cooling a precipitate
  9. customformed
  10. filtrationthis was filtered
  11. washwashed with H2O