HRID1095745

反应详情

EQUATION

反应方程式

HRID 1095745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of potassium carbonate (0.351 g, 2.54 mmol), pyridin-3-ylboronic acid (68.6 mg, 0.558 mmol), 7-bromoimidazo[1,2-a]pyridine (0.100 g, 0.508 mmol) and tetrakis(triphenylphosphine)palladium (0) (29.3 mg, 0.025 mmol) in 6.5 ml of a 1:1:4.5 mixture of water:dimethylformamide:acetonitrile was degassed thoroughly under a nitrogen atmosphere, and heated at 60° C. for 18 hours. The reaction mixture was poured in water (50 ml) and extracted with dichloromethane and EtOAc. The combined organic extracts were dried over anhydrous sodium sulfate and concentrated to afford a solid. The solid was purified by silica gel chromatography (eluting with 6% MeOH-chloroform) to afford the desired compound (74.1 mg, 75% yield). MS APCI (+) m/z 196.3 (M+1) detected.

WORKUP

后处理

  1. customdimethylformamide:acetonitrile was degassed thoroughly under a nitrogen atmosphere
  2. additionThe reaction mixture was poured in water (50 ml)
  3. extractionextracted with dichloromethane and EtOAc
  4. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customto afford a solid
  7. customThe solid was purified by silica gel chromatography (eluting with 6% MeOH-chloroform)