反应详情

Aluminum chloride (2.05 g., 0.0154 mole) was added to cold (-30° C.) tetrahydrofuran (75 ml.). Sodium azide was added and the mixture heated under reflux for 40 minutes. Ethyl 2-cyano-3-(5,6,7,8-tetrahydro-1-isoquinolylamino)-acrylate (3.33 g., 0.0123 mole) was added and the mixture heated under reflux for 20 hours. The cooled mixture was diluted with water (100 ml.) and acidified with concentrated hydrochloric acid. The precipitate was collected, washed with water, dried and recrystallized from 2-methoxyethanol to give the title compound (0.625 g., 19%), m.p. 290°-292° C. (decomp.).

1. temperaturethe mixture heated
2. temperatureunder reflux for 40 minutes
3. temperaturethe mixture heated
4. temperatureunder reflux for 20 hours
5. customThe precipitate was collected
6. washwashed with water
7. customdried
8. customrecrystallized from 2-methoxyethanol