反应详情

To a solution of 4-(1,3-dioxolan-2-yl)benzonitrile (2 g, 0.01 mol) in dry pyridine (50 mL) and TEA (5.75 g, 0.057 mol) was passed H2S gas (freshly generated) for 1 h with stirring at RT. The reaction mixture was diluted with water (100 mL), extracted with diethyl ether (100 mL), washed with brine (50 mL) and dried. The solvent was removed under vacuum and the crude product was purified by column chromatography over silica gel (PetEther/EtOAc, 3/7) to give 4-(1,3-dioxolan-2-yl)benzenecarbothioamide (1.9 g, 86%) as yellow solid. TLC (PetEther/EtOAc 3/7), Rf=0.35

1. customfor 1 h
2. extractionextracted with diethyl ether (100 mL)
3. washwashed with brine (50 mL)
4. customdried
5. customThe solvent was removed under vacuum
6. customthe crude product was purified by column chromatography over silica gel (PetEther/EtOAc, 3/7)