反应详情

The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+.

1. additionAfter the addition
2. temperatureThe mixture was warmed
3. temperatureto reflux
4. stirringstirred for 1 h
5. temperatureThe reaction was cooled to 0° C.
6. customto quench
7. customthe reaction
8. filtrationThe material was filtered
9. washthe residue was washed with EtOAc
10. concentrationthe filtrate was concentrated under reduced pressure
11. customdirectly to the next reaction