反应详情

A mixture of 18.1 g. (0.055 mole) of diethyl {[(1-phenyl-5-pyrazolyl)amino]methylene}malonate and 150 ml of diethyl phthalate was heated at 240-250° for 1 hour. The mixture was chilled and diluted with hexane. Chilling and filtering gave crystals which were washed with hexane and with hexane-ethanol (1:1) to give 11 g. (70%) of off white crystals, m.p. 149-150° C. From a similar small scale run 1.75 g. was recrystallized from 110 ml. of ethanol to give 1.58 g. of off white crystals, m.p. 149-150° C.

1. additionA mixture of 18.1 g
2. temperatureThe mixture was chilled
3. temperatureChilling
4. filtrationfiltering
5. customgave crystals which
6. washwere washed with hexane and with hexane-ethanol (1:1)
7. customto give 11 g
8. customwas recrystallized from 110 ml
9. customof ethanol to give 1.58 g