反应详情

A solution of 3,6-dichloro4H-thieno[3,2-e]-1,2,4-thiadiazine 1,1-dioxide (386 mg, 1.5 mmol) in 1-methylcyclopropylamine (1.0 g, 14 mmol) was stirred for 24 h at 85° C. in a sealed flask. The cooled solution was concentrated in vacuo and the residue was stirred with ethyl acetate (1-2 ml) and filtered. The white precipitate was stirred in 4M hydrochloric acid (5 ml) for 2 h and then filtered off and chromatographed on silica gel with ethyl acetate to give 112 mg (26%) of the pure title compound; mp 251-252° C. dec; 1H-NMR (DMSO-d6): δ0.65-0.79 (m, 4H), 1.36 (s, 3H), 7.11 (s, 1H), 7.82 (br s, 1H), 10.78 (br s, 1H); MS: m/e 291/293 (M+); (C9H10N3Cl1O2S2) calc. C, 37.05; H, 3.45; N, 14.40; found C, 36.96; H, 3.53; N, 14.15.

1. concentrationThe cooled solution was concentrated in vacuo
2. filtrationfiltered
3. stirringThe white precipitate was stirred in 4M hydrochloric acid (5 ml) for 2 h
4. filtrationfiltered off
5. customchromatographed on silica gel with ethyl acetate