HRID644501

反应详情

EQUATION

反应方程式

HRID 644501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 7-iodo-1-phenyl-5-trifluoromethylbenzimidazole (370 mg, 1 mmol), benzeneboronic acid (180 mg, 1.5 mmol), potassium carbonate (700 mg, 5 mmol) and tetrakis(triphenylphosphine)palladium(0) (29 mg, 0.025 mmol) in a mixture of water (5 ml) and dimethoxyethane (10 ml) was stirred at reflux overnight. The cooled mixture was partitioned between water and ethyl acetate. The organic phase was collected, washed with brine, dried and concentrated under reduced pressure. Recrystallisation from methanol afforded the product as an off-white solid (160 mg, 47%), m/z, 339.1 (M+H)+.

WORKUP

后处理

  1. temperatureat reflux overnight
  2. customThe cooled mixture was partitioned between water and ethyl acetate
  3. customThe organic phase was collected
  4. washwashed with brine
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customRecrystallisation from methanol