反应详情

To 30 g (167 mmole) of O-ethyl dichlorothiophosphate in 100 ml of tetrahydrofuran (THF) cooled to -70° C. was added a solution of sodium propoxide (from 7.4 g of 60% NaH (184 mmole) and 11 g (176 mmole) of 1-propanol) in 50 ml of THF. After warming to room temperature over 2 hours, the THF was removed in vacuo and the residue was partitioned between 50 ml diethyl ether, 50 ml hexanes, and 25 ml cold water. The organic layer was dried over magnesium sulfate, concentrated in vacuo, and distilled (bp 45-50° C. 1 torr) yielding 20 g of the title compound, an oil. nmr 1.0 t 3H, 1.4 t 3H, 1.8 sextet 2H, 4.4 m 4H.

1. customthe THF was removed in vacuo
2. customthe residue was partitioned between 50 ml diethyl ether, 50 ml hexanes, and 25 ml cold water
3. dry with materialThe organic layer was dried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. distillationdistilled (bp 45-50° C. 1 torr)