Diethyl chlorophosphate → 1-[Ethoxy(isothiocyanato)phosphoryl]oxyethane

To a mixture of 8.02 g of dry sodium thiocyanate in 100 ml of dry toluene at 0° C., under a nitrogen atmosphere is added 13.1 ml (16.6 g) of diethyl phosphorchloridate dropwise with stirring. The mixture is warmed to ambient temperature and stirred 20 hours. The mixture is filtered through a pad of Celite and the pad is washed with two 50 ml portions of toluene. The filtrate is washed with 50 ml of ice cold 10% sodium bicarbonate solution, 50 ml of ice water and dried over anhydrous magnesium sulfate. The mixture is filtered and the filtrate used without further purification in subsequent reaction.

1. stirringstirred 20 hours
2. filtrationThe mixture is filtered through a pad of Celite
3. washthe pad is washed with two 50 ml portions of toluene
4. washThe filtrate is washed with 50 ml of ice cold 10% sodium bicarbonate solution, 50 ml of ice water
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe mixture is filtered
7. customthe filtrate used without further purification in subsequent reaction

ORD record

ord-5077741d62f14f00bf812f57aeebf227

Source dataset

uspto-grants-1979_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04137310