反应详情

温度

60 °C

A solution of 71a/71b (212.3 mg, 0.4626 mmol) in 1:1 THF:MeOH (2.3 mL, 0.2 M) was treated with hydrazine monohydrate (224.4 μL, 4.626 mmol) and heated to 60° C. overnight. The reaction was cooled to RT, and the solids were filtered off. The filtrate was concentrated to dryness and taken up in EtOAc (30 mL). The EtOAc solution was washed with saturated NaHCO3 (2×30 mL) and brine (1×30 mL). The organics were isolated, dried (Na2SO4), filtered and concentrated. The crude product was purified by SiO2 chromatography eluting with a 1-25% gradient of MeOH/3% NH4OH in DCM to afford 110 mg (72%) of 73a/73b as a clear oil containing approximately a 1:1 mixture of diastereomers.

1. temperatureThe reaction was cooled to RT
2. filtrationthe solids were filtered off
3. concentrationThe filtrate was concentrated to dryness
4. washThe EtOAc solution was washed with saturated NaHCO3 (2×30 mL) and brine (1×30 mL)
5. customThe organics were isolated
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude product was purified by SiO2 chromatography
10. washeluting with a 1-25% gradient of MeOH/3% NH4OH in DCM