HRID334044

反应详情

EQUATION

反应方程式

HRID 334044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a mixture of 2.90 g (12.6 mmol) 6-bromo-pyridine-2-carboxylic acid ethyl ester in 25 mL toluene was added 3.00 g (29.7 mmol) cyclopropylboronic acid and 5.50 g (25.9 mmol) potassium phosphate followed by 700 mg (0.957 mmol) 1,1′-bis(diphenylphosphino)-ferrocenedichloropalladium(II). The reaction mixture was stirred at 100° C. for 8 h. 1.00 g (9.90 mmol) of cyclopropylboronic acid and 1.50 g (7.07 mmol) of potassium phosphate were added and the mixture was stirred at 100° C. for 5 h. The reaction mixture was filtered through Celite, and washed with DCM and the solvent was evaporated in vacuo. The crude material was purified by flash chromatography (PE/EtOAc=4/1→2/1).

WORKUP

后处理

  1. stirringthe mixture was stirred at 100° C. for 5 h
  2. filtrationThe reaction mixture was filtered through Celite
  3. washwashed with DCM
  4. customthe solvent was evaporated in vacuo
  5. customThe crude material was purified by flash chromatography (PE/EtOAc=4/1→2/1)