反应详情

To a solution of methyl 2-(dimethylamino)-N-[[(methylamino)carbonyl]oxy]-2-oxoethanimidothioate (3.29 g, 0.015 mole) in dry pyridine 15 ml was added at one time thionyl chloride (1.79 g, 0.015 mole) at -30°. The mixture was allowed to come to room temperature and then stirred for 15 minutes. The mixture was cooled to 0° and O,O-diethyl methylphosphoramidothioate (2.75 g, 0.01 mole) was added. The mixture was allowed to come to room temperature for 1 hour, poured into ice water and extracted with benzene. The benzene solution was washed with water 4 times and then dried over anhydrous sodium sulfate. The benzene was removed under reduced pressure to give a crude product of the formula below. ##STR40##

1. customto come to room temperature
2. temperatureThe mixture was cooled to 0°
3. waitto come to room temperature for 1 hour
4. extractionextracted with benzene
5. washThe benzene solution was washed with water 4 times
6. dry with materialdried over anhydrous sodium sulfate
7. customThe benzene was removed under reduced pressure