反应详情

A solution of 10.3 g of 1-(2-diisopropylaminoethyl)isatin, 5.1 g of semicarbazide hydrochloride and 3.7 g of sodium acetate in 150 ml of a mixture of ethanol and water (2:1) was stirred for 17 hours at room temperature. The yellow precipitates were collected by filtration and washed with aqueous ethanol. The filtrate and the washed the aqueous ethanol solution were combined and concentrated under reduced pressure. An aqueous sodium bicarbonate solution was added to the residue. The yellow precipitates were collected by filtration and washed with dichloromethane. The yellow precipitates were combined and recrystallized from aqueous methanol to obtain 9.3 g of (E)-1-(2-diisopropylaminoethyl)isatin 3-semicarbazone having a melting point of 193°-196° C.

1. customThe yellow precipitates
2. filtrationwere collected by filtration
3. washwashed with aqueous ethanol
4. washThe filtrate and the washed the aqueous ethanol solution
5. concentrationconcentrated under reduced pressure
6. additionAn aqueous sodium bicarbonate solution was added to the residue
7. customThe yellow precipitates
8. filtrationwere collected by filtration
9. washwashed with dichloromethane
10. customThe yellow precipitates
11. customrecrystallized from aqueous methanol