HRID244701

反应详情

EQUATION

反应方程式

HRID 244701 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium hydride (299 mg, 7.48 mmol) was added to a stirred solution of 4-bromo-6-fluoro-1H-indole (800 mg, 3.74 mmol) in DMF (20 ml) that had been cooled in an ice bath to 0° C. and placed under nitrogen. The mixture was stirred for 5 mins before 4-nitrobenzenesulfonyl chloride (911 mg, 4.11 mmol) was added. The mixture was stirred at 0° C. for 1 hour. The resultant orange/brown solution was poured into stirring water (40 ml). The mixture was rapidly stirred for 30 mins. The resulting brown suspension was collected by filtration, washed with water and dried in a vacuum oven at 50° C. overnight to give a pale brown solid, which was purified by Flashmaster II, on a silica cartridge (100 g) using a gradient of ethylacetate and cyclohexane to afford the title compound as a white solid.

WORKUP

后处理

  1. additionwas added
  2. additionThe resultant orange/brown solution was poured
  3. stirringThe mixture was rapidly stirred for 30 mins
  4. filtrationThe resulting brown suspension was collected by filtration
  5. washwashed with water
  6. customdried in a vacuum oven at 50° C. overnight
  7. customto give a pale brown solid, which
  8. customwas purified by Flashmaster II, on a silica cartridge (100 g)