反应详情

To 300 ml of 1,4 dioxane in a round-bottom flask was added 11.6 g (0.1 mole) of dimethylglyoxime. When the solid had completely dissolved, 22.9 g (0.2 mole) of methanesulfonyl chloride was added. The mixture was stirred and 20.2 g (0.2 mole) triethylamine was added dropwise. The reaction mixture was stirred for 51/2 hours during which time a precipitate was formed. The dioxane was removed by evaporation under reduced pressure. The residue was stirred in ice water, then filtered. The solid product was dissolved in dichloromethane and dried over anhydrous sodium sulfate. The slurry was filtered and the solvent was removed in a rotary evaporator. The solid residue was stirred in cold ethanol, then filtered and dried in a vacuum oven, giving 21.05 g (77% yield) of di-(methanesulfonyl)-dimethylglyoxime with mp 169-172° C.

1. dissolutionWhen the solid had completely dissolved
2. stirringThe reaction mixture was stirred for 51/2 hours during which time a precipitate
3. customwas formed
4. customThe dioxane was removed by evaporation under reduced pressure
5. stirringThe residue was stirred in ice water
6. filtrationfiltered
7. dissolutionThe solid product was dissolved in dichloromethane
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationThe slurry was filtered
10. customthe solvent was removed in a rotary evaporator
11. stirringThe solid residue was stirred in cold ethanol
12. filtrationfiltered
13. customdried in a vacuum oven