反应详情

To 2A (7.20 g, 28.3 mmol) in THF (190 mL) was added 1 N LiOH (94 mL). The reaction was stirred for 1 h at rt, then was heated gradually to 65° C. After cooling to rt, the THF was removed under reduced pressure. The remaining solution was cooled to 0° C. and acidified to pH 1 with 1N HCl. The product was extracted with CH2Cl2, and the organic layer was washed with brine, dried (MgSO4), filtered and concentrated to provide 2B as a clear oil (6.30 g). LC-MS: 241.08 (M+H)+.

1. temperaturewas heated gradually to 65° C
2. temperatureAfter cooling to rt
3. customthe THF was removed under reduced pressure
4. temperatureThe remaining solution was cooled to 0° C.
5. extractionThe product was extracted with CH2Cl2
6. washthe organic layer was washed with brine
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated