反应详情

温度

20 °C

3-(5-Tetrazolyl)xanthone (1.0 g) was dissolved in concentrated sulphuric acid (10.0 ml) and the resulting solution cooled to below 15° C. Potassium nitrate (0.50 g) was added in small portions over 10 min. with cooling to maintain the temperature between 10° and 15° C. and the reaction mixture was then stirred at 20° C. for 1 hr. The reaction mixture was poured on to ice and the precipitated product filtered off, washed with water and recrystallised from dimethylformamide. The crystallised product was washed with methanol and dried at 156° C./20 mm Hg to yield 0.78 g, mpt. ca. 280° C. with decomposition.

1. temperaturethe resulting solution cooled to below 15° C
2. temperaturewith cooling
3. temperatureto maintain the temperature between 10° and 15° C.
4. additionThe reaction mixture was poured on to ice
5. filtrationthe precipitated product filtered off
6. washwashed with water
7. customrecrystallised from dimethylformamide
8. washThe crystallised product was washed with methanol
9. customdried at 156° C./20 mm Hg
10. customto yield 0.78 g, mpt
11. customca. 280° C.