反应详情

温度

25 °C

Methanol (50 mL) was placed into a round bottom flask and 3-cyano-4-isobutoxy benzothioamide (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 for about 30 minutes. The mass was then filtered and washed with methanol. The wet solid was dried at about 70° C. to a constant weight to yield 5.0 g of the title compound. Purity by HPLC: 84.9%.

1. temperatureThe mixture was heated
2. temperatureto reflux
3. temperaturemaintained until reaction completion
4. temperaturemaintained for about 30 minutes
5. filtrationThe mass was then filtered
6. washwashed with methanol
7. customThe wet solid was dried at about 70° C. to a constant weight