反应详情

温度

0 °C

20 ml of water and then, at 0° C., 22 mg (0.6 mmol) of sodium borohydride were added to a solution of 500 mg (1.1 mmol) of 8.2 in 50 ml of ethanol. After stirring at 0° C. for 40 min, the reaction mixture was concentrated in vacuo, the residue was heated at 50° C. for 12 h in 30 ml of 6 N hydrochloric acid/THF (1:1) and the reaction mixture was allowed to stand overnight at room temperature. The mixture was extracted with dichloromethane and the organic phase was dried over sodium sulfate. After filtration, the solvent was removed in vacuo, and the residue was treated with water and freeze-dried. 440 mg of crude 8.3 were obtained, which was employed in the next synthesis step without further purification.

1. concentrationthe reaction mixture was concentrated in vacuo
2. temperaturethe residue was heated at 50° C. for 12 h in 30 ml of 6 N hydrochloric acid/THF (1:1)
3. waitto stand overnight at room temperature
4. extractionThe mixture was extracted with dichloromethane
5. dry with materialthe organic phase was dried over sodium sulfate
6. filtrationAfter filtration
7. customthe solvent was removed in vacuo
8. additionthe residue was treated with water
9. customfreeze-dried
10. custom440 mg of crude 8.3 were obtained
11. customwhich was employed in the next synthesis step without further purification