反应详情

温度

25 °C

Toluene (50 mL) was placed into a round bottom flask and 3-cyano-4-isobutoxybenzothioamide (5.0 g) was added, followed by addition of ethyl-2-chloroacetoacetate (4.25 g). The mixture was heated to reflux and maintained until reaction completion. After the reaction was completed, the mass was cooled to about 25° C. and maintained at that temperature for about 20 minutes. The reaction mass was then filtered and the solid was washed with toluene (10 mL). The wet solid was dried at about 75° C. to a constant weight to yield 4.0 g of the title compound. Purity by HPLC: 99.41%.

1. temperatureThe mixture was heated
2. temperatureto reflux
3. temperaturemaintained until reaction completion
4. temperaturemaintained at that temperature for about 20 minutes
5. filtrationThe reaction mass was then filtered
6. washthe solid was washed with toluene (10 mL)
7. customThe wet solid was dried at about 75° C. to a constant weight