反应详情

温度

0 °C

A mixture of Phosphoric acid di-tert-butyl ester (1 g, 0.0048 mol), NaHCO3 (0.806 g, 0.0096 mol), tetra butyl ammonium hydrogen sulphate (0.163 g, 0.00048 mol), water (40 ml) and DCM (25 ml) were taken. The mixture was cooled to 0° C. and stirred at that temperature for 20 minutes. Chloromethyl chlorosulphatc, (0.943 g, 0.0057 mol) in DCM (15 ml) was added to it at 0° C. The reaction mixture allowed to warm to room temperature and stirred for 18 hours. The organic layer was separated and aqueous layer was extracted with DCM (30 ml). The organic layer was washed with brine (60 ml) solution and dried over Na2SO4. The organic layer was evaporated to obtain Phosphoric acid di-tert-butyl ester chloromethyl ester as colorless oil (0.79 g, 64%).

1. temperatureto warm to room temperature
2. stirringstirred for 18 hours
3. customThe organic layer was separated
4. extractionaqueous layer was extracted with DCM (30 ml)
5. washThe organic layer was washed with brine (60 ml) solution
6. dry with materialdried over Na2SO4
7. customThe organic layer was evaporated