反应详情

To a 25 mL press resistant vial which contained a suspension of LiAlH4 (100 mg, 3 mmol) in anhydrous THF (15 mL) was added the product from step 1 (120 mg, 0.3 mmol) at −78° C. The reaction mixture was allowed to warm to rt and stir at rt for 2 h then was heated to 78° C. and stirred at 78° C. for 24 h. After cooled to 5° C., 1 eq of water was added to the mixture which was followed by addition of 1 eq of 15% NaOH and then 3 eq of water. The solid which formed was filtered out and washed with THF water (2×20 mL). The combined organic solvent was removed under vacuo to obtain the crude product which was purified by recrystallization with ether-EtOAc-hexane to afford the title product, (50 mg, 57%);LCMS; 99%, ESI+ Calcd: 308.4 m/z, found: 309.7 m/z (M+1);

1. temperaturethen was heated to 78° C.
2. stirringstirred at 78° C. for 24 h
3. temperatureAfter cooled to 5° C.
4. customThe solid which formed
5. filtrationwas filtered out
6. washwashed with THF water (2×20 mL)
7. customThe combined organic solvent was removed under vacuo
8. customto obtain the crude product which
9. customwas purified by recrystallization with ether-EtOAc-hexane