反应详情

温度

50 °C

To a solution of oxetan-3-one (600 mg, 8.33 mmol) and 2-methylpropane-2-sulfinamide (1.01 g, 8.33 mmol) in tetrahydrofuran (14 mL), titanium ethoxide (3.45 mL, 16.65 mmol) was added. The mixture was stirred at 50° C. overnight. The reaction mixture was poured over brine. The suspension was filtered through celite and washed with ethyl acetate. The solution was partitioned between ethyl acetate and brine. The organics were dried (Na2SO4), filtered and concentrated. The residue was purified by column chromatography on silica (0-70% ethyl acetate in hexanes) to afford 2-methyl-N-(oxetan-3-ylidene)propane-2-sulfinamide (692 g, 3.20 mmol, 38% yield) as a clear oil. MS ESI: [M+H]+ m/z 176.1.

1. filtrationThe suspension was filtered through celite
2. washwashed with ethyl acetate
3. customThe solution was partitioned between ethyl acetate and brine
4. dry with materialThe organics were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by column chromatography on silica (0-70% ethyl acetate in hexanes)