反应详情

To 50 ml of 6 N hydrochloric acid was added 11.8 g of 2-amino-4-chloro-5-sulfamylaniline and 10.4 g of 2-methylbenzyl cyanide. The reaction was refluxed for 22 hours and then concentrated in vacuo to a solid which was then added with stirring to 200 ml of 38% ammonium hydroxide. Filtration provided the free base as a semi-gum which was dissolved in 500 ml of methanol. The methanol solution was brought to a boil, charcoal added, and boiling continued for five minutes. Upon cooling, the suspension was filtered through Celite and the filtrate concentrated in vacuo to yield a solid, m.p. 226°-230°.

1. temperatureThe reaction was refluxed for 22 hours
2. concentrationconcentrated in vacuo to a solid which
3. additionwas then added
4. filtrationFiltration
5. customprovided the free base as a semi-gum which
6. additionadded
7. temperatureUpon cooling
8. filtrationthe suspension was filtered through Celite
9. concentrationthe filtrate concentrated in vacuo
10. customto yield a solid, m.p. 226°-230°