反应详情

370 mg of 8alpha-(3,3-diethylureido)-2,6-dimethyl-ergoline-13-carbaldehyde (1 mmol) is dissolved in 50 ml of tetrahydrofuran and reduced with 200 mg of lithium aluminum hydride at room temperature for 1 hour. The mixture is cooled off in an ice bath and mixed in succession with 0.2 ml of water, 0.2 ml of 15% sodium hydroxide solution and 0.6 ml of water, the precipitate is filtered off and the filtrate is evaporated to dryness. The residue is chromatographed on silica gel with dichloromethane/methanol. 243 mg of alcohol, which crystallizes from ethyl acetate, is isolated. Yield 166 mg (44% of theory), [α]D =+6° (0.5% in chloroform).

1. temperatureThe mixture is cooled off in an ice bath
2. filtrationthe precipitate is filtered off
3. customthe filtrate is evaporated to dryness
4. customThe residue is chromatographed on silica gel with dichloromethane/methanol
5. custom243 mg of alcohol, which crystallizes from ethyl acetate
6. customis isolated