HRID1511822

反应详情

EQUATION

反应方程式

HRID 1511822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1.00 g of 3-chloropyrido[2,3-b]pyrazin-6-ylamine (5.54 mmol), 743 mg of phenylboronic acid (6.09 mmol), 640 mg of tetrakis(triphenylphosphine)palladium(0) (0.55 mmol) and 1.76 g of sodium carbonate (16.6 mmol) were initially charged in 100 ml of dimethylformamide/water (1:1) under nitrogen as a protective gas and stirred at 80° C. for 2 h. Once the reaction had ended, the mixture was filtered off with suction and the filtrate was poured onto 800 ml of distilled water. The aqueous phase was extracted repeatedly with ethyl acetate. The organic phase was freed of solvents under reduced pressure. The resulting solid was purified by means of column chromatography on silica gel (dichloromethane/methanol eluent). This gave a yellow solid.

WORKUP

后处理

  1. filtrationthe mixture was filtered off with suction
  2. additionthe filtrate was poured onto 800 ml of distilled water
  3. extractionThe aqueous phase was extracted repeatedly with ethyl acetate
  4. customThe resulting solid was purified by means of column chromatography on silica gel (dichloromethane/methanol eluent)
  5. customThis gave a yellow solid