HRID1951651
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled to r.t.
- filtrationfiltered through a pad of silica gel
- concentrationThe filtrate was concentrated under vacuum
- dissolutionthe crude product was dissolved in 100 ml of ethanol
- temperatureThe resulting mixture was heated
- temperatureto reflux for 10 h
- additiondiluted with 50 ml of water
- temperatureAfter cooling to r.t.
- filtrationsolid was collected by filtration
- customair-dried