反应详情

A solution of 750 mg. (2.13 mmol) of the end product of Example 9 in 50 ml. methanol in a glass bomb was cooled to 3° and saturated with ammonia. The glass bomb was then sealed and the reaction heated to 70° with stirring, for 16 hours. After cooling to 5°, the bomb was opened, the contents transferred to a r.b. flask and concentrated in vacuo. Recrystallization was acetone/hexane yielded end product, mp 216°-218°. An analytical sample was prepared by an additional recrystallization from acetone/hexane and obtained as pale yellow needles: mp 217°-219°.

1. customThe glass bomb was then sealed
2. temperaturethe reaction heated to 70°
3. temperatureAfter cooling to 5°
4. concentrationflask and concentrated in vacuo
5. customRecrystallization
6. customAn analytical sample was prepared by an additional recrystallization from acetone/hexane
7. customobtained as pale yellow needles