反应详情

温度

60 °C

The product obtained in Step C (3 mmol), dissolved in 1,1,2,2-tetrachloroethane (30 ml), is added dropwise to a solution of aluminium chloride (10 mmol) in the same solvent (20 ml) under nitrogen. The reaction mixture is heated at 60° C., with stirring, until the reaction has ceased and it is then poured into a mixture of ice (10 g) and concentrated HCl (0.3 ml); stirring is continued for one hour. The aqueous phase is extracted twice with chloroform; the combined organic phases are then dried over magnesium sulphate and concentrated under reduced pressure. The residue is chromatographed on silica gel to yield the title product.

1. stirringstirring
2. extractionThe aqueous phase is extracted twice with chloroform
3. dry with materialthe combined organic phases are then dried over magnesium sulphate
4. concentrationconcentrated under reduced pressure
5. customThe residue is chromatographed on silica gel