反应详情

A stirred solution of the product of Step 228b (274 mg, 0.590 mmol) and NH2NH2.H2O (114 mg, 2.27 mmol) in MeOH (10 mL) was heated to reflux for 2.5 h. After this time, the reaction mixture was cooled to rt then concentrated under reduced pressure. The resulting residue was triturated with a mixture of CH2Cl2/hexanes (1:1) and the solid was filtered off. The filtrate was concentrated under reduced pressure and dried under high vacuum to afford the title compound as a white foam (182 mg, 93%). ESI MS (M+H) 329.

1. temperatureto reflux for 2.5 h
2. concentrationthen concentrated under reduced pressure
3. customThe resulting residue was triturated with a mixture of CH2Cl2/hexanes (1:1)
4. filtrationthe solid was filtered off
5. concentrationThe filtrate was concentrated under reduced pressure
6. customdried under high vacuum