反应详情

50 ml of a solution of 15% by weight of BF3 in acetic acid are added rapidly to a suspension of 26.3 g (0.1 mole) of 5-cyano-10-nitro-5H-dibenz[b,f]azepine in a mixture of 260 ml of chlorobenzene and 130 ml of acetic acid and, while heating gently, a clear yellow solution is obtained. The reaction mixture is stirred for 10 minutes and then 40 g of iron powder are added in one portion. While stirring well, 100 ml of water are added dropwise in the course of 30 minutes, the temperature increasing to 65°. By external heating the temperature is maintained at 60°-65° for two hours, and the inorganic material is filtered off and washed with chlorobenzene and acetic acid. After separating the chlorobenzene phase, this is washed with water until crystallisation of the product begins. The product is concentrated in vacuo and the residue is taken up in 100 ml of methanol. After suction-filtering and washing with a little methanol, 5-carbamoyl-10-oxo-10,11-dihydro-5H-dibenz[b,f]azepine is obtained, which according to the IR spectrum is identical to authentic material.

1. temperaturewhile heating gently
2. customa clear yellow solution is obtained
3. stirringWhile stirring well
4. temperaturethe temperature increasing to 65°
5. temperatureBy external heating the temperature
6. temperatureis maintained at 60°-65° for two hours
7. filtrationthe inorganic material is filtered off
8. washwashed with chlorobenzene and acetic acid
9. customAfter separating the chlorobenzene phase
10. washthis is washed with water until crystallisation of the product
11. concentrationThe product is concentrated in vacuo
12. filtrationAfter suction-filtering
13. washwashing with a little methanol