反应详情

Ethyl 3-bromopropionate (9.05 g) in acetone (70 ml) was added to 3-(5-tetrazolyl)thioxanthone-10,10-dioxide (15.6 g) and sodium hydroxide (2.0 g) in water (15 ml). The mixture was boiled under reflux for 8 hr. On cooling the ester product crystallised out and was filtered off, washed with dilute sodium bicarbonate solution, and recrystallised from ethanol, m.p. 143°-145° C. The ester (4.5 g) was boiled with a mixture of concentrated hydrochloric acid (40 ml) and acetic acid (120 ml) for 3 hr. On cooling, 3-((2-carboxyethyl)-5-tetrazolyl)thioxanthone-10,10-dioxide crystallised out and was filtered off and washed with water, m.p. 206°-207° C.

1. temperatureunder reflux for 8 hr
2. customcrystallised out
3. filtrationwas filtered off
4. washwashed with dilute sodium bicarbonate solution
5. customrecrystallised from ethanol, m.p. 143°-145° C
6. additionThe ester (4.5 g) was boiled with a mixture of concentrated hydrochloric acid (40 ml) and acetic acid (120 ml) for 3 hr
7. temperatureOn cooling
8. custom3-((2-carboxyethyl)-5-tetrazolyl)thioxanthone-10,10-dioxide crystallised out
9. filtrationwas filtered off
10. washwashed with water, m.p. 206°-207° C.