反应详情

温度

25 °C

Potassium hydroxide (23 mg, 0.406 mmol) was added to a solution of example 25 (10 mg, 0.0203 mmol) in 3-methyl-3-pentanol (2 mL) and the mixture was heated under reflux for 16 hours. The solution was cooled to 25° C. and potassium hydroxide (23 mg, 0.406 mmol) was added and the solution was heated under reflux for an additional 24 hours. The reaction mixture was then cooled to room temperature, concentrated in vacuo and the residue was purified by column chromatography on silica gel, eluting with ethyl acetate:methanol:0.88 ammonia, 95:5:0.5. to afford the title compound as a colourless gum in 68% yield, 7 mg.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 16 hours
3. temperaturethe solution was heated
4. temperatureunder reflux for an additional 24 hours
5. temperatureThe reaction mixture was then cooled to room temperature
6. concentrationconcentrated in vacuo
7. customthe residue was purified by column chromatography on silica gel
8. washeluting with ethyl acetate