HRID1951651

反应详情

EQUATION

反应方程式

HRID 1951651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A mixture of 7-bromo-1H-indole-2,3-dione (4.5 g), Cs2CO3 (10 g) and 1-bromomethyl-4-trifluoromethylbenzene (5 g) in 50 ml of DMF was stirred at 55° C. for 6 h. The reaction mixture was cooled to r.t., diluted with 100 ml of 1:1 hexane/EtOAc and filtered through a pad of silica gel. The filtrate was concentrated under vacuum and the crude product was dissolved in 100 ml of ethanol and 10 ml of 50% aqueous solution of hydrazine. The resulting mixture was heated to reflux for 10 h and diluted with 50 ml of water. After cooling to r.t., solid was collected by filtration and air-dried to give the title compound as a white solid (5.2 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to r.t.
  2. filtrationfiltered through a pad of silica gel
  3. concentrationThe filtrate was concentrated under vacuum
  4. dissolutionthe crude product was dissolved in 100 ml of ethanol
  5. temperatureThe resulting mixture was heated
  6. temperatureto reflux for 10 h
  7. additiondiluted with 50 ml of water
  8. temperatureAfter cooling to r.t.
  9. filtrationsolid was collected by filtration
  10. customair-dried