反应详情

Sodium (0.69 g, 30 mmol) was added to about 50 ml of ethanol and allowed to react. The mixture was allowed to cool and then 4.0 g (9.8 mmol) of N-(2,6-dichloro-3-methylphenyl)-7-chloro-5-methyl-1,2,4-triazolo[1,5-a]pyrimidine-2-sulfonamide was added with stirring. After 15 minutes to starting material remained by thin layer chromatographic analysis although complete solution was never attained. The mixture was acidified with 6N hydrochloric acid and concentrated under reduced pressure. The residue was triturated with water and the solid removed by filtration and washed with water. It was then dissolved in aqueous sodium hydroxide using a minimum amount of the base and the aqueous solution was twice extracted with ether and acidified with 6N hydrochloric acid. The solid that formed was collected by filtration, washed with water, and dried. This was extracted with about 500 ml of boiling chloroform. The chloroform solution was concentrated to about 150 ml and allowed to cool to form a precipitate which was collected by filtration and dried to obtain 1.7 g (42 percent of theory) of the title compound as a white solid, m.p. 228°-9° C.

1. customto react
2. temperatureto cool
3. concentrationconcentrated under reduced pressure
4. customThe residue was triturated with water
5. customthe solid removed by filtration
6. washwashed with water
7. dissolutionIt was then dissolved in aqueous sodium hydroxide using a minimum amount of the base
8. extractionthe aqueous solution was twice extracted with ether
9. customThe solid that formed
10. filtrationwas collected by filtration
11. washwashed with water
12. customdried
13. extractionThis was extracted with about 500 ml of boiling chloroform
14. concentrationThe chloroform solution was concentrated to about 150 ml
15. temperatureto cool
16. customto form a precipitate which
17. filtrationwas collected by filtration
18. customdried