反应详情

温度

80 °C

To a partial suspension of 2-sulfamoyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (3.05 g, 14 mmol) in ethyl acetate (200 ml) was added activated manganese dioxide (3.0 g). This mixture was warmed to 80° C. Every two hours an additional 3.0 g of activated manganese dioxide was added until 12 g total had been added. This mixture was filtered hot and the collected manganese dioxide was re-extracted with hot ethyl acetate. The combined ethyl acetate extracts were evaporated to give 2.1 g of crude product. This material was purified by chromatography on silica gel eluting with a gradient 0-5% methanol/ethyl acetate. Recrystallization from ethyl acetate gave pure product (0.8 g, 26.5% yield); m.p. 161°-164° C.

1. additionhad been added
2. filtrationThis mixture was filtered hot
3. extractionthe collected manganese dioxide was re-extracted with hot ethyl acetate
4. customThe combined ethyl acetate extracts were evaporated
5. customto give 2.1 g of crude product
6. customThis material was purified by chromatography on silica gel eluting with a gradient 0-5% methanol/ethyl acetate
7. customRecrystallization from ethyl acetate