反应详情

A solution of 4.3 g (14 mmol) of 4-(phenylsulfonyl)benzyl bromide and 30 g (0.1 mole) of tris-trimethylsilylphosphite was heated at 120° C. for 18 hours. The excess tris-trimethylsilylphosphite was distilled off under reduced pressure. The residue was dissolved in 200 ml of 9:1 tetrahydrofuran/water and was allowed to stand at room temperature for 18 hours. The tetrahydrofuran was evaporated and the resulting solids were filtered and washed with water to give 1.4 g of product; m.p. 217-219° C.

1. distillationThe excess tris-trimethylsilylphosphite was distilled off under reduced pressure
2. dissolutionThe residue was dissolved in 200 ml of 9:1 tetrahydrofuran/water
3. customThe tetrahydrofuran was evaporated
4. filtrationthe resulting solids were filtered
5. washwashed with water