反应详情

A mixture of 4-chloro-3-nitrophenyl methyl sulfone (4 g, 17 mmole) and N,N-dimethylethylenediamine (3.3 g, 37 mmole) in DMSO (20 ml) was stored at 75° C. for 1 hour and poured into crushed ice. The yellow solid precipitate was collected by filtration and was dissolved in ethyl acetate. The organic phase was washed with water-brine mixture twice and brine, dried over sodium sulfate, and evaporated under reduced pressure to give the sulfone (22) (3.8 g, 78%) as a yellow solid. A pure sample (m.p. 130°-131° C.) was obtained by recrystallization from ethyl acetate.

1. additionpoured
2. custominto crushed ice
3. filtrationThe yellow solid precipitate was collected by filtration
4. dissolutionwas dissolved in ethyl acetate
5. washThe organic phase was washed with water-brine mixture twice
6. dry with materialbrine, dried over sodium sulfate
7. customevaporated under reduced pressure