反应详情

Ethyl 2-amino-4-phenyl-thiophene-3-carboxylate (2 g, 8.087 mmol) and trifluoroacetamidine (4.531 g, 40.44 mmol) were combined in ethanol (20 mL) and heated to reflux overnight. Further trifluoroacetamidine (4.531 g, 40.44 mmol) was added and the reaction heated to reflux for a further 18 hours. The reaction mixture was allowed to cool to room temperature. The resulting precipitate was filtered off, washed with ethanol (5 mL) and dried in vacuo at 40° C. to afford 5-phenyl-2-(trifluoromethyl)-3H-thieno[2,3-d]pyrimidin-4-one (1.195 g). LCMS: purity 99%, RT=4.11 min, M+1=297.

1. temperatureheated
2. temperatureto reflux overnight
3. temperaturethe reaction heated
4. temperatureto reflux for a further 18 hours
5. filtrationThe resulting precipitate was filtered off
6. washwashed with ethanol (5 mL)
7. customdried in vacuo at 40° C.