反应详情

A mixture of 2.5 g of 2-(4-t-butoxycarbonylaminophenyl)-3-oxobutyronitrile, 20 ml of ethanol and 1.4 g of 2,2-diethoxyethylhydrazine was heated under reflux for 2 hours. 20 ml of 4N hydrogen chloride in dioxane were added, and then the whole mixture was heated under reflux for a further 30 minutes. After the mixture had been cooled, ethyl acetate was added to precipitate crystals. These crystals were collected by filtration and recrystallized from ethanol to give 1.4 g of the title compound as pale brown plates melting at 180°-190° C.

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. temperaturethe whole mixture was heated
4. temperatureunder reflux for a further 30 minutes
5. temperatureAfter the mixture had been cooled
6. customto precipitate crystals
7. filtrationThese crystals were collected by filtration
8. customrecrystallized from ethanol