反应详情

At -10° C., 0.5 g (1.6 mmol) of N-butyl-N-(1,1-dioxo-2,3-dihydro-1H-benzo[b]thiophen-3-yl)methanesulfonamide (Example 5) was dissolved in 5 ml of concentrated sulfuric acid and admixed with 0.15 g (1.8 mmol) of sodium nitrate, and the mixture was stirred at RT for 20 h. The reaction mixture was poured into 50 ml of ice-water, stirred for 30 minutes, filtered off with suction, washed neutral with water and dried under reduced pressure. This procedure gave 0.5 g of N-butyl-N-(6-nitro-1,1-dioxo-2,3-dihydro-1H-benzo[b]thiophen-3-yl)-methanesulfonamide; m.p. 52-55° C.

1. stirringstirred for 30 minutes
2. filtrationfiltered off with suction
3. washwashed neutral with water
4. customdried under reduced pressure