反应详情

A mixture of 9.0 g of 2-amino-4-chloro-5-sulfamyl aniline, 14.1 g of butyric acid, and 40.3 ml of a 15% hydrochloric acid solution was refluxed for 6 hours and then concentrated in vacuo to a solid. The solid was dissolved in hot methanol, treated with charcoal, boiled ten minutes, and filtered. Concentration in vacuo provided a solid which was then added portionwise to 200 ml of concentrated ammonium hydroxide. The free base was then recrystallized from acetonitrile to yield 4.5 g of pink crystals, m.p. 230°-234°.

1. temperaturewas refluxed for 6 hours
2. concentrationconcentrated in vacuo to a solid
3. dissolutionThe solid was dissolved in hot methanol
4. additiontreated with charcoal
5. waitboiled ten minutes
6. filtrationfiltered
7. concentrationConcentration in vacuo
8. customprovided a solid which
9. customThe free base was then recrystallized from acetonitrile