反应详情

A solution of 18.02 g (50.5 mmol) of dimethyl 4,4′-[2-(hydroxymethyl)butane-1,4-diyl]dibenzoate in 350 ml of dichloromethane is mixed with 13.07 g (60.6 mmol) of pyridinium chlorochromate (PCC) and stirred at room temperature for 12 hours. After conversion is complete, about 60 g of silica gel are added, and the solvent is removed in vacuo to dryness. The residue is purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 5:1→4:1). 14.73 g (41.46 mmol, 82% of theory) of a colourless oil are obtained.

1. additionabout 60 g of silica gel are added
2. customthe solvent is removed in vacuo to dryness
3. customThe residue is purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 5:1→4:1)
4. custom14.73 g (41.46 mmol, 82% of theory) of a colourless oil are obtained