反应详情

A solution of 3-(dimethylamino)-1-[4-(trifluoromethyl)phenyl]-2-propen-1-one (may be prepared as described in Intermediate 2) (1.49 g, 6.13 mmol) in dichloromethane (DCM) (6 ml) was cooled in an ice-water bath before the dropwise addition of POCl3 (0.571 ml, 6.13 mmol). The ice-water bath was removed and the reaction mixture stirred at room temperature for 3 hours. The solvent was removed under vacuum to yield a solid. To the solid was then added to an ice-cold solution of sodium perchlorate (3.75 g, 30.6 mmol) in water (8 mL) and diethyl ether (2 mL). The resulting suspension was stirred in an ice-water bath for 20 minutes. The solid was then collected by filtration, washed with ice-cold water (4 mL), dried by suction for 40 minutes then dried overnight under vacuum to yield the title compound as a solid (2.39 g.

1. customThe ice-water bath was removed
2. customThe solvent was removed under vacuum
3. customto yield a solid
4. stirringThe resulting suspension was stirred in an ice-water bath for 20 minutes
5. filtrationThe solid was then collected by filtration
6. washwashed with ice-cold water (4 mL)
7. customdried by suction for 40 minutes
8. customthen dried overnight under vacuum