反应详情

21.5 g (0.12 mol) of 4-chlorophenylhydrazine hydrochloride was suspended in 150 mL of methanol, 5 mL of concentrated hydrochloric acid was added, and the mixture was heated at reflux, which gave a clear, yellow-brown solution. To this solution was added dropwise 11.5 g (0.12 mol) of dimethylaminoacrylonitrile over a period of 30 minutes. After 1.5 h at reflux, most of the solvent was removed under vacuum. The remaining residue was taken up in 40 mL of dimethylformamide, and 9 mL of concentrated ammonia solution was added at room temperature. The resulting white precipitate was filtered off and discarded. The clear filtrate was used in Step 10.2 without further purification.

1. temperaturethe mixture was heated
2. temperatureat reflux
3. customwhich gave a clear, yellow-brown solution
4. temperatureAfter 1.5 h at reflux, most of the solvent
5. customwas removed under vacuum
6. addition9 mL of concentrated ammonia solution was added at room temperature
7. filtrationThe resulting white precipitate was filtered off
8. customThe clear filtrate was used in Step 10.2 without further purification