反应详情

A mixture of 120 ml toluene, 80 ml hexane, 24.2 g acetylpyridine, 24.2 g of diphenylhydrazine hydrochloride, and 30 g of anhydrous sodium acetate was stirred and heated at reflux in a flask equipped with a water separator until no more water was being collected (about 2 hours). The reaction mixture was filtered, and the filtrate was distilled under aspirator vacuum at 60° C. The residue was stirred with 100 ml of methanol with cooling to keep temprature between -10° and -20° C. The resulting solid was collected, washed with 100 ml of cold methanol, and was dried in vacuo to give 43 g of acetylpyridine diphenylhydrazone, mp 84° C. λmax in methanol is 358 nm; absorptivity is 6.7×103.

1. temperatureheated
2. temperatureat reflux in a flask
3. customwas being collected (about 2 hours)
4. filtrationThe reaction mixture was filtered
5. distillationthe filtrate was distilled under aspirator vacuum at 60° C
6. stirringThe residue was stirred with 100 ml of methanol
7. temperaturewith cooling
8. customto keep temprature between -10° and -20° C
9. customThe resulting solid was collected
10. washwashed with 100 ml of cold methanol
11. customwas dried in vacuo