反应详情

To a solution of ethyl 2-amino-5-(4-fluorophenyl)thiophene-3-carboxylate (0.3 g, 1.13 mmol) and acetonitrile (0.56 ml, 11.3 mmol) in dioxane (4 ml) was added 4M HCl in dioxane (4 ml). The mixture was stirred at room temperature overnight. The solvents were removed under reduced pressure. The residue was diluted with water and made alcaline with a saturated aqueous sodium bicarbonate solution. The precipitate was filtered off, washed with water and dried. The crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1) to yield the title compound as a white solid (0.29 g, 81%).

1. customThe solvents were removed under reduced pressure
2. additionThe residue was diluted with water
3. filtrationThe precipitate was filtered off
4. washwashed with water
5. customdried
6. customThe crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1)