HRID244710

反应详情

EQUATION

反应方程式

HRID 244710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium Hydride (0.667 g, 16.66 mmol) was added portion-wise over 15 mins to a stirred solution of 5-bromo-1H-pyrazolo[3,4-b]pyridine (3 g, 15.15 mmol, available from ChemGenx LLC) in N,N-dimethylformamide (30 ml) that had been cooled in an ice bath to 0° C. and placed under nitrogen. The mixture was stirred for 20 mins, until hydrogen evolution ceased, and then benzenesulfonyl chloride (2.148 ml, 16.66 mmol) was added. The mixture was stirred for 18 hours, letting the ice melt over this time. The solution was poured into stirring water (10 ml) and rapidly stirred for 15 mins. The mixture was then poured onto water (70 ml) and filtered. The orange solid obtained was dried in the vacuum oven for 18 h to afford the title compound (3.86 g).

WORKUP

后处理

  1. additionThe solution was poured
  2. stirringrapidly stirred for 15 mins
  3. additionThe mixture was then poured onto water (70 ml)
  4. filtrationfiltered
  5. customThe orange solid obtained
  6. customwas dried in the vacuum oven for 18 h