反应详情

A solution of 3,6-dichloro-4H-thieno[3,2-e]-1,2,4-thiadiazine 1,1-dioxide (1.0 g, 3.9 mmol) and cumylamine (1.06 g, 7.8 mmol) in ethanol (6 ml) was stirred for 31 h at 120° C. in a sealed flask. The cooled solution was concentrated in vacuo and the residue dissolved in 1N sodium hydroxide (50 ml) followed by treatment with decolourising charcoal. After filtration, the clear solution was acidified to pH <2 with 4M hydrochloric acid and the precipitate was filtered off and recrystallised from ethanol to give 278 mg (20%) of the title compound; mp ca. 360° C. (decomposes gradually above 200° C.); 1H-NMR (DMSO-d6): δ1.68 (s, 6H), 7.12 (s, 1H), 7.17-7.41 (m, 6H), 10.72 (br s, 1H); MS: m/e 355/357 (M+); (C14H14ClN3O2S2) calc C, 47,25; H, 3.97; N, 11.81; found C, 46.82; H, 3.96; N, 11.62.

1. concentrationThe cooled solution was concentrated in vacuo
2. dissolutionthe residue dissolved in 1N sodium hydroxide (50 ml)
3. filtrationAfter filtration
4. filtrationthe precipitate was filtered off
5. customrecrystallised from ethanol