反应详情

To dipropyl hydroxymethylphosphine-oxide (Ref. U.S. Pat. No. 5,272,128) (16.4 g, 0.1 mol) in anhydrous ether (200 mL) at 0° C., was added p-toluenesulfonyl chloride (19.1 g, 0.1 mol), triethyl amine (27.8 mL, 0.2 mol). The reaction was stirred at room temperature over night. The ether solution was decanted, and the precipitate was washed in a filter funnel with ˜1 L ether until HPLC found no product. Combined ether layer were concentrated. The crude product was purified on silica gel chromatography with 8% MeOH/DCM.

1. customThe ether solution was decanted
2. washthe precipitate was washed in a filter funnel with ˜1 L ether until HPLC
3. concentrationCombined ether layer were concentrated
4. customThe crude product was purified on silica gel chromatography with 8% MeOH/DCM