反应详情

温度

70 °C

3-Methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate (1.0 g) was added to hydrazine hydrate (0.8 ml) and the mixture was heated to 70° C. for 30 min. After cooling, the reaction mixture was supplemented with methanol (10 ml) and the solvents were removed by distillation under reduced pressure. The residue was dissolved in NaOH 2M (20 ml), treated with charcoal, filtered, and the filtrate was adjusted to pH 6-7 with HCl 1M. The precipitate so obtained was collected by filtration, washed with water an dried (yield: 0.8 g); m.p. 290°-292° C. (Compound 1).

1. temperatureAfter cooling
2. customthe solvents were removed by distillation under reduced pressure
3. dissolutionThe residue was dissolved in NaOH 2M (20 ml)
4. additiontreated with charcoal
5. filtrationfiltered
6. customThe precipitate so obtained
7. filtrationwas collected by filtration
8. washwashed with water
9. customan dried (yield: 0.8 g)