反应详情

4-Cyanothioxanthone-10,10-dioxide (1.35g), sodium azide (0.39g) ammonium chloride (0.32g) and dimethylsulphoxide were heated together at 125°- 130° C. for 6.5 hr. The mixture was cooled, poured into dilute hydrochloric acid and the precipitated product filtered off. It was warmed with 1% sodium bicarbonate solution, filtered, and the filtrate acidified with dilute hydrochloric acid. 4-(5-Tetrazolyl)thioxanthone-10,10-dioxide was filtered off and recrystallised from acetic acid, m.p. 271° C. with decomposition. Found: C 53.50%; H 2.70%; N 18.04%. C14H8N4O3S requires C 53.85%; H 2.58%; N 17.95%.

1. temperatureThe mixture was cooled
2. filtrationthe precipitated product filtered off
3. temperatureIt was warmed with 1% sodium bicarbonate solution
4. filtrationfiltered
5. filtration4-(5-Tetrazolyl)thioxanthone-10,10-dioxide was filtered off
6. customrecrystallised from acetic acid, m.p. 271° C. with decomposition