反应详情

0.62 g (6.2 mmol) of neutral alumina and 1.3 g (6.1 mmol) of pyridinium chlorochromate are added to a solution of 1.05 g (3.05 mmol) of the compound from Example 2 in 50 ml of methylene chloride and the mixture is stirred at room temperature for 1 hour. It is filtered through kieselguhr and then washed with 200 ml of methylene chloride. The methylene chloride phase is concentrated in vacuo and the residue is chromatographed on a column (100 g of silica gel, 70-230 mesh, diameter 3.5 cm) using ethyl acetate/petroleum ether 1:9.

1. filtrationIt is filtered through kieselguhr
2. washwashed with 200 ml of methylene chloride
3. concentrationThe methylene chloride phase is concentrated in vacuo
4. customthe residue is chromatographed on a column (100 g of silica gel, 70-230 mesh, diameter 3.5 cm)