反应详情

温度

60 °C

A solution of isopropylhydrazine hydrochloride (1.06 g, 9.6 mmol), (3-oxo-propyl)-carbamic acid benzyl ester (2.0 g, 9.6 mmol), and Et3N (3.9 g, 38.4 mmol) in isopropanol (30 mL) was heated to reflux. After 3 h, the solution was treated with 2-[3-(4-fluoro-phenyl)-2-nitro-allyl]-[1,3]dioxolane (2.2 g, 8.7 mmol) and stirred at 60° C. for 18 h. The mixture was cooled to rt and concentrated. The residue was partitioned between EtOAc and water. The organic layer was separated, dried (MgSO4), and concentrated. Purification by FCC gave the title compound.

1. temperatureThe mixture was cooled to rt
2. concentrationconcentrated
3. customThe residue was partitioned between EtOAc and water
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customPurification by FCC