反应详情

35 G (0.28 mole) of caprolactim-methyl-ether were added dropwise over the course of 15 minutes at 5°C, while stirring and cooling, to a solution of 36 g (0.25 mole) of 3-chlorophenylhydrazine in 250 ml of glacial acetic acid; the red-brown clear solution was kept at 0° to 5°C for a further 2 hours and then for 2 hours at 20°C and excess glacial acetic acid was distilled off in a water-pump vacuum. On fractional distillation in vacuo of the residue which remained, 56 g (94.3% of theory) of caprolactam-(3-chlorophenylhydrazone) were obtained; it was a light viscous oil of boiling point 215° to 220°C/3 mmHg, which solidified to crystals.

1. waitfor 2 hours at 20°C
2. distillationexcess glacial acetic acid was distilled off in a water-pump vacuum
3. distillationOn fractional distillation in vacuo of the residue which