反应详情

300 G of hydrogen chloride gas were introduced into a solution of 1,000g(7 moles) of 3-chlorophenylhydrazine and 980 g (7.7 moles) of caprolactim-methyl-ether in 4,000 ml of methanol at 10° to 20°C while stirring and cooling with an ice bath, and the reaction mixture was kept for a further hour at 20°C, raised to the reflux temperature and kept at 65°C for 11/2 hours. After cooling, the crystals which had separated out were filtered off and further crystal fractions were isolated by concentrating the mother liquors under reduced pressure. After recrystallization from 2 parts of methanol, 1,845 g (96% of theory) of caprolactam-(3-chlorophenylhydrazone) hydrochloride were obtained as colorless crystals of melting point 280° to 282°C.

1. temperaturecooling with an ice bath
2. waitthe reaction mixture was kept for a further hour at 20°C
3. temperatureraised to the reflux temperature
4. customkept at 65°C for 11
5. custom2 hours
6. temperatureAfter cooling
7. customthe crystals which had separated out
8. filtrationwere filtered off
9. customfurther crystal fractions were isolated
10. concentrationby concentrating the mother liquors under reduced pressure
11. customAfter recrystallization from 2 parts of methanol