反应详情

Sodium (0.46 g) was dissolved in ethanol (20 ml) and 3-(5-tetrazolyl)thioxanthone-10,10-dioxide (6.24g) was added. Ethyl bromoacetate (3.34 g) was added to the mixture, which was boiled under reflux for 1.5 hr. The ester intermediate was deposited during this time, and after cooling was filtered off, washed with water and dried, m.p. 194°-195° C. The ester was boiled with concentrated hydrochloric acid (40 ml) and acetic acid (120 ml) for 2 hr. On cooling 3-(2-carboxymethyl-5-tetrazolyl)thioxanthone-10,10-dioxide crystallised out, and was filtered off, recrystallised from acetic acid, and dried, m.p. 252° C. with decomposition.

1. temperatureunder reflux for 1.5 hr
2. temperatureafter cooling
3. filtrationwas filtered off
4. washwashed with water
5. customdried
6. temperatureOn cooling 3-(2-carboxymethyl-5-tetrazolyl)thioxanthone-10,10-dioxide
7. customcrystallised out
8. filtrationwas filtered off
9. customrecrystallised from acetic acid
10. customdried