反应详情

1-Methyl-4,6-dichloroisatin (4.0 g) was suspended in dry ethanol (40 ml), hydrazine (9 ml) was added and the mixture was refluxed in 6 h. The mixture was then added slowly at 70° C. to a solution of sodium (1.74 g) in dry ethanol (80 ml) and refluxed overnight. The reaction mixture was cooled to room temperature, water (50 ml) was added and the volume was reduced to about one third by evaporation. The mixture was then poured onto icewater (1000 ml) and acidified with 6M HCl (pH=1). The precipitate was filtered off washed with water and dried to afford 3.27 g (87%) of (43). M.p. 144°-145° C.

1. temperaturethe mixture was refluxed in 6 h
2. temperaturerefluxed overnight
3. customthe volume was reduced to about one third by evaporation
4. additionThe mixture was then poured onto icewater (1000 ml)
5. filtrationThe precipitate was filtered off
6. washwashed with water
7. customdried