反应详情

Into the solution of the 2-chloro-1,3,2-oxathiaphospholane of Example 1 (28.5 g, 0.2 mol) in n-pentane (300 mL) was added dropwise, at room temperature, with stirring, N,N-diisopropylamine (40.5 g, 0.4 mol). After 0.5 h diisopropylamine hydrochloride was removed by filtration, solvent was evaporated under reduced pressure, and the product was distilled. The fraction collected at 70° C./0.1 mmHg was shown by means of 31P NMR to be homogeneous. Yield: 70%. 31P NMR: δ147.8 ppm (benzene). MS: m/z 207 (M-, E.I., 15 eV).

1. customAfter 0.5 h diisopropylamine hydrochloride was removed by filtration, solvent
2. customwas evaporated under reduced pressure
3. distillationthe product was distilled
4. customThe fraction collected at 70° C./0.1 mmHg