HRID38814

反应详情

EQUATION

反应方程式

HRID 38814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

To a solution of 6-bromo-1H-indazole-4-carbonitrile (5 g, 22.52 mmol) in N,N-dimethylformamide (50 ml) was added, in portions, sodium hydride (1.351 g, 33.8 mmol) and the mixture stirred at 20° C. for 15 mins then cooled to 0° C. when benzenesulfonyl chloride (3.16 ml, 24.77 mmol) was added dropwise. The mixture was stirred at 20° C. for 18 h then concentrated in vacuo and the residue partitioned between water (100 ml) and dichloromethane (100 ml). The organic layer was separated by hydrophobic frit and evaporated in vacuo to give the title compound as a yellow solid (7.94 g).

WORKUP

后处理

  1. additionwas added dropwise
  2. stirringThe mixture was stirred at 20° C. for 18 h
  3. concentrationthen concentrated in vacuo
  4. customthe residue partitioned between water (100 ml) and dichloromethane (100 ml)
  5. customThe organic layer was separated by hydrophobic frit
  6. customevaporated in vacuo