反应详情

温度

50 °C

A solution of (4R,5S)-2,2-dimethyl-5-[(4-methylphenyl)sulfonyl]oxy-1,3-dioxolan-4-yl 4-methyl-1-benzenesulfonate (5.07 g, 10.8 mmol) in a tetrahydrofuran (50 ml) −10% perchloric acid water (50 ml) mixed solvent was stirred at 50° C. for 7 hours. The tetrahydrofuran was distilled off under reduced pressure, extraction was performed with ethyl acetate and the extract was washed with brine. After drying with anhydrous magnesium sulfate, the solvent was distilled off to yield a crude product which was then purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (5.14 g). This was used without further purification for the following reaction.

1. distillationThe tetrahydrofuran was distilled off under reduced pressure, extraction
2. washthe extract was washed with brine
3. dry with materialAfter drying with anhydrous magnesium sulfate
4. distillationthe solvent was distilled off
5. customto yield a crude product which
6. customwas then purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)