反应详情

温度

50 °C

To a 250 mL round-bottomed flask was added 2-methylpropane-2-sulfinamide (3.36 g, 27.8 mmol) followed by tetraethoxytitanium (11.64 ml, 55.5 mmol) to a tetrahydrofuran (69.4 ml) solution of oxetan-3-one (2 g, 27.8 mmol) at room temperature. The mixture was stirred at 50° C. for 5 hours, cooled and poured into brine. The suspension was filtered through a pad of diatomaceous earth eluting with ethyl acetate. The organics were combined, dried with sodium sulfate, filtered and concentrated under vacuum. The residue was purified by regular phase flash column chromatography to give the title compound.

1. temperaturecooled
2. filtrationThe suspension was filtered through a pad of diatomaceous earth
3. washeluting with ethyl acetate
4. dry with materialdried with sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue was purified by regular phase flash column chromatography