反应详情

7-Chloro-3-methylsulfinyl-4H-1,2,4-benzothiadiazine 1,1-dioxide (0.25 g) and 2-aminopyridine (0.25 g) in 3-chlorotoluene (5 mL) was heated at 150° C. for 1 h. After cooling, the white precipitate was collected by filtration and washed with diethylether. The insoluble material was dissolved in 1M NaOH (20 mL), treated with charcoal, filtered, and the filtrate was adjusted to pH 3 with 6N HCl. The precipitate was collected by filtration, washed with water, dissolved in hot DMF (15 mL), mixed with an equal volume of distilled water and cooled. The white precipitate was collected by filtration, washed with water and dried (yield: 0.12 g); m.p. >310° C.

1. temperatureAfter cooling
2. filtrationthe white precipitate was collected by filtration
3. washwashed with diethylether
4. dissolutionThe insoluble material was dissolved in 1M NaOH (20 mL)
5. additiontreated with charcoal
6. filtrationfiltered
7. filtrationThe precipitate was collected by filtration
8. washwashed with water
9. dissolutiondissolved in hot DMF (15 mL)
10. additionmixed with an equal volume of distilled water
11. temperaturecooled
12. filtrationThe white precipitate was collected by filtration
13. washwashed with water
14. customdried (yield: 0.12 g)