[NH2:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7](=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:15](=O)([O:17]CC)[NH2:16]>[Cl-].[Zn+2].[Cl-]>[C:8]1([C:7]2[C:6]3[CH:5]=[CH:4][S:3][C:2]=3[NH:1][C:15](=[O:17])[N:16]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1A mixture of 10.0 g of 2-amino-3-benzoylthiophene, 16.57 g of ethyl carbamate and 1.00 g of zinc chloride is heated at 200°C for 1 hour. After cooling, the reaction mixture is washed with chloroform, then with water, and filtered to give a solid of 4-phenyl-1,2-dihydrothieno[2,3-d]pyrimidin-2-one. Recrystallization from a mixture of ethanol and dimethylformamide gives crystals having a melting point of 247° - 249°C.
Wird geladen…