反应详情

A stirred mixture of Intermediate 104 (0.50 g), sodium methanethiolate (0.35 g), potassium carbonate (0.43 g) and copper (I) iodide (0.025 g) in dry N,N-dimethylformamide (3 ml) was heated at 100° under nitrogen for 18 h. The mixture was cooled, poured into water (50 ml) and stirred for 15 min. The solid material was filtered off, dried in vacuo at 80° for 2 h, and boiled in ethanol:water 15:1 (50 ml) for 30 min. The insoluble material was filtered off, and the filtrate evaporated to dryness to give the title compound as a pale yellow solid (0.163 g).

1. temperaturewas heated at 100° under nitrogen for 18 h
2. temperatureThe mixture was cooled
3. filtrationThe solid material was filtered off
4. customdried in vacuo at 80° for 2 h
5. waitboiled in ethanol:water 15:1 (50 ml) for 30 min
6. filtrationThe insoluble material was filtered off
7. customthe filtrate evaporated to dryness