HRID38486

反应详情

EQUATION

反应方程式

HRID 38486 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

N,N-diisopropylethylamine (4.14 ml, 23.71 mmol) was added to a stirred mixture of 1-acetyl-5-bromo-3-methyl-1H-indazole (2.00 g, 7.90 mmol), DPPF (0.657 g, 1.185 mmol) and Pd(OAc)2 (0.266 g, 1.185 mmol) in DMF (20 ml)-MeOH (5 ml) at room temperature and the mixture was stirred in CO atomospher (1 atm) at 90° C. overnight. After the mixture was cooled and the CO gas was removed by N2 gas, the mixture was filtered through celite pad and the filtrate was evaporated under reduced pressure. The residue was purified by silicagel column chromatography (hexane/EtOAc) to give intended compound as a pale brown solid.

WORKUP

后处理

  1. temperatureAfter the mixture was cooled
  2. customthe CO gas was removed by N2 gas
  3. filtrationthe mixture was filtered through celite pad
  4. customthe filtrate was evaporated under reduced pressure
  5. customThe residue was purified by silicagel column chromatography (hexane/EtOAc)
  6. customto give