反应详情

Into 1.5 l of ethanol were dispersed 118 g of ethylβ-anilino-β-ethoxy acrylate and 94 g of p-sulfophenylhydrazine, and 150 g of triethylamine and glacial acetic acid were successively dropped thereinto while heating (95°-100° C.) and stirring. After heating (95°-100° C.) and stirring for 5 hours, the reaction solution was concentrated under reduced pressure. To the residue so concentrated were added 50 ml of water and 120 ml of ethanol containing 35% by wt. hydrogen chloride to provide a uniform solution. This uniform solution was allowed to stand in a refrigerator for one day and one night. The crystals of the objective compound which precipitated had a melting point of 290° to 291° C. and weighed 145 g.

1. additionwere successively dropped
2. temperaturewhile heating (95°-100° C.)
3. temperatureAfter heating (95°-100° C.)
4. stirringstirring for 5 hours
5. concentrationthe reaction solution was concentrated under reduced pressure
6. concentrationTo the residue so concentrated
7. additionwere added 50 ml of water and 120 ml of ethanol containing 35% by wt. hydrogen chloride
8. customto provide a uniform solution
9. customThe crystals of the objective compound which precipitated