反应详情

温度

80 °C

Sodium cyanate (0.28 g, 4.32 mmol) in water (6 ml) was added dropwise to a stirred solution of 2 (1.0 g, 2.16 mmol) in water (30 ml) and 1N HCl (4.3 ml) at 80° C. After 2 h at 80° C. the mixture was cooled and extracted with dichloromethane (3×20 ml) and the extract dried (MgSO4) and evaporated in vacuo. The residue was purified by column chromatography on silica gel [dichloromethane/methanol (97:3)] to obtain the title compound (0.70 g, 64%) as a yellow solid.

1. extractionextracted with dichloromethane (3×20 ml)
2. dry with materialthe extract dried (MgSO4)
3. customevaporated in vacuo
4. customThe residue was purified by column chromatography on silica gel [dichloromethane/methanol (97:3)]