反应详情

温度

80 °C

Intermediate 67a (633 mg, 2.62 mmol) was suspended in EtOH (5 mL) and hydrazine hydrate (50-60%, 5 mL) in a microwave vial fitted with a stirrer bar and sealed with a crimped septum, and heated to 80° C. for 18 h. The reaction was cooled, and partitioned between H2O and EtOAc. The organic layer was separated, and the aqueous extracted again with EtOAc. The combined organics were dried over MgSO4, and concentrated in vacuo to afford the title compound as a colorless oil (593 mg, 89%). LCMS (Method 3) Rt 0.41 and 1.71 min, m/z 276.2 [M+Na].

1. customsealed with a crimped septum
2. temperatureThe reaction was cooled
3. custompartitioned between H2O and EtOAc
4. customThe organic layer was separated
5. extractionthe aqueous extracted again with EtOAc
6. dry with materialThe combined organics were dried over MgSO4
7. concentrationconcentrated in vacuo