反应详情

1.8 g of Grignard magnesium are placed in 19 ml of anhydrous ethyl ether in a round-bottomed flask equipped with a mechanical stirrer, and under a stream of nitrogen. A mixture of 8.9 ml of 4-bromotrifluoromethylbenzene in 46 ml of anhydrous ethyl ether is then added. The mixture is stirred for one hour, followed by addition of a solution of 5.7 g of 4,6-dichloro-1H-indole-2,3-dione in 100 ml of anhydrous THF. The mixture is stirred at room temperature for 4 hours 30 minutes. Water is added and the resulting mixture is extracted with ethyl acetate. The organic phase is separated out and dried over Na2SO4, filtered and evaporated under vacuum. The residue is taken up in ethyl acetate and washed with 1N sodium hydroxide solution. The organic phase is dried over Na2SO4, filtered and evaporated under vacuum. The solid is taken up in ethyl ether and filtered off. 4.7 g of expected product are obtained.

1. customequipped with a mechanical stirrer
2. additionis then added
3. stirringThe mixture is stirred at room temperature for 4 hours 30 minutes
4. extractionthe resulting mixture is extracted with ethyl acetate
5. customThe organic phase is separated out
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. customevaporated under vacuum
9. washwashed with 1N sodium hydroxide solution
10. dry with materialThe organic phase is dried over Na2SO4
11. filtrationfiltered
12. customevaporated under vacuum
13. filtrationfiltered off