反应详情

127 G (1 mole) of caprolactim-methyl-ether were added dropwise over the course of 30 minutes to a mixture of 144.5 g (1 mole) of phenylhydrazine hydrochloride and 700 ml of anhydrous ethanol at -10°C, while stirring well and cooling; the mixture was kept for a further hour at -10°C, then for 2 hours at room temperature and for 30 minutes at the reflux temperature. After cooling, the mixture was filtered and further crystal fractions were isolated by concentrating the mother liquor under reduced pressure. Recrystallization from 5 parts of ethanol yielded 220 g (92% of theory) of caprolactam-phenylhydrazone hydrochloride as almost colorless crystals of melting point 244° to 246°C (with decomposition).

1. temperaturecooling
2. waitthe mixture was kept for a further hour at -10°C
3. waitfor 30 minutes at the reflux temperature
4. temperatureAfter cooling
5. filtrationthe mixture was filtered
6. customfurther crystal fractions were isolated
7. concentrationby concentrating the mother liquor under reduced pressure
8. customRecrystallization from 5 parts of ethanol