反应详情

10.3 g (48 mmol) of pyridinium chlorochromate and 4.9 g (48 mmol) of neutral alumina are added to a solution of 3.8 g (12 mmol) of the compound from Example 4 in 100 ml of methylene chloride p.a. and the mixture is stirred for 1 h at room temperature. The mixture is filtered over kieselgur with suction and washed with 300 ml of methylene chloride. The methylene chloride phase is concentrated in vacuo and the residue is chromatographed on a column (150 g of silica gel 70-230 mesh, φ3.5 cm, using ethyl acetate/petroleum ether 2:8).

1. filtrationThe mixture is filtered over kieselgur with suction
2. washwashed with 300 ml of methylene chloride
3. concentrationThe methylene chloride phase is concentrated in vacuo
4. customthe residue is chromatographed on a column (150 g of silica gel 70-230 mesh, φ3.5 cm, using ethyl acetate/petroleum ether 2:8)