反应详情

3,4-Diaminobenzoic acid (20 g, 0.13 mol) was suspended in formic acid (120 ml) while cooling. After that hydrochloric acid (12 ml) was added. An obtained reaction mass was agitated for 24 hours at a room temperature. Reaction mixture was filtered through fiber glass filter. Then filter cake was dissolved in water (400 ml), pH was adjusted to 2.0 with ammonia solution and reaction mass was agitated overnight. Resulting suspension was filtered, pH of filtrate was adjusted to 3.0 with ammonia solution and reaction mass was agitated for two hours. Precipitate was filtered and dried at ˜100° C. H1NMR (Brucker Avance-300, DMSO-d6, δ, ppm): 7.695 (d, H, CHAr(7)); 7.877 (dd, H, CHAr(6)); 8.25 (d, H, CHAr(4)); 8.44 (s, H, (s, H, CHAr(2)); 12.82 (s, 2H, NH, COOH). Yield was 11.3 g (54%).

1. temperaturewhile cooling
2. customAn obtained reaction mass
3. customReaction mixture
4. filtrationwas filtered through fiber glass
5. filtrationfilter
6. filtrationThen filter cake
7. dissolutionwas dissolved in water (400 ml)
8. custompH was adjusted to 2.0 with ammonia solution and reaction mass
9. stirringwas agitated overnight
10. customResulting suspension
11. filtrationwas filtered
12. custompH of filtrate was adjusted to 3.0 with ammonia solution and reaction mass
13. stirringwas agitated for two hours
14. filtrationPrecipitate was filtered
15. customdried at ˜100° C