反应详情

A mixture comprising 30 g (312 mmol) of sulfamide, 27.5 g (312 mmol) of N-methyl-1,3-propanediamine and 300 ml of dry pyridine was refluxed overnight at 130° C. The mixture was left to cool, and then pyridine was distilled off under reduced pressure. To the residue, 200 ml of chloroform was added and insoluble substance was filtered off. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (CHCl3) and then subjected to distillation under reduced pressure to obtain 36.2 g of 2-methyl-tetrahydro-1,2,6-thiadiazine-1,1-dioxide (boiling point: 130°-133° C./0.23 mmHg).

1. waitThe mixture was left
2. temperatureto cool
3. distillationpyridine was distilled off under reduced pressure
4. additionTo the residue, 200 ml of chloroform was added
5. filtrationinsoluble substance was filtered off
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel column chromatography (CHCl3)
8. distillationsubjected to distillation under reduced pressure