反应详情

A solution of N,N diethyl methanesulfonamide (4.7 g) in tetrahydrofuran (50 ml) was stirred at 20° C and treated with butyllithium in hexane (2.6 N, 27.9 ml) and diethyl chlorophosphate (5.2 ml). The cooling bath was removed and the mixture was stirred for 1.5 hours and poured onto ice. The resulting mixture was saturated with sodium bicarbonate, extracted with methylene chloride and the organic phase was washed with water, dried with sodium sulfate and magnesium sulfate, filtered and concentrated in vacuo to give diethyl [[(diethylamino)sulfonyl]methyl]-phosphonate.

1. customThe cooling bath was removed
2. additionpoured onto ice
3. extractionextracted with methylene chloride
4. washthe organic phase was washed with water
5. dry with materialdried with sodium sulfate and magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo