反应详情

To a solution of the intermediate from step A (2.15 g, 8.45 mmol) in ethanol (100 mL) was added benzyl hydrazine hydrochloride (1.8 g, 9.22 mmol) and HOAc (10 mL). The reaction mixture was stirred at room temperature for 16 hours and then refluxed at 70° C. for 30 minutes. The reaction was cooled to room temperature and concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with water, saturated NaHCO3, and brine. The organic layer was dried over anhydrous Na2SO4 filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2) using 30% ethyl acetate-hexanes to give the desired product (1.64 g) a brown oil.

1. temperaturerefluxed at 70° C. for 30 minutes
2. temperatureThe reaction was cooled to room temperature
3. concentrationconcentrated in vacuo
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with water, saturated NaHCO3, and brine
6. dry with materialThe organic layer was dried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was purified by flash chromatography (SiO2)