反应详情

温度

4 °C

A mixture of 5 (7.23 g, 2.94 mmol) and pyridinium p-toluenesulfonate (0.74 g, 2.94 mmol) in acetone (150 mL) was stirred in a cold room at 4° C. for 5 days. The mixture was neutralized with sodium bicarbonate solution, and diluted with toluene. After evaporation of acetone, the residue was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, and dried over sodium sulfate. Filtration and concentration gave 9.22 g of an oily material, which was purified by column chromatography (silica gel 60 g, 4-16% ethyl acetate in n-hexane) to give 6.16 g (quantitative) of 6, as a pale yellow oil.

1. customAfter evaporation of acetone
2. additionthe residue was diluted with water
3. extractionextracted with ethyl acetate
4. washThe combined organic layers were washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationFiltration and concentration