反应详情

50 ml of a solution of 15% by weight of BF3 in acetic acid (=0.11 mole) are added to a suspension of 26.3 g (0.1 mole) of 5-cyano-10-nitro-5H-dibenz[b,f]azepine in 100 ml of acetic acid at room temperature. In the course of this the temperature rises slowly to 34° with complete dissolution of the starting material. 30 ml of water are added at 30° in the course of 5 minutes, resulting in a further increase in temperature to 37°. At this temperature 40 g of iron powder are added in portions over a period of 20 minutes, the temperature being maintained at 65°-70° by occasional cooling. After the exothermic reaction has subsided, stirring is continued for a further 15 minutes and then inorganic material is filtered off and washed three times with a little acetic acid. The total filtrate is added dropwise, while stirring well, to 11/2 l of water and, after stirring for 2 hours, the resulting precipitate is filtered off and washed neutral with water. After drying in vacuo at 60°, 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. dissolutionIn the course of this the temperature rises slowly to 34° with complete dissolution of the starting material
2. customresulting in
3. temperaturea further increase in temperature to 37°
4. temperaturethe temperature being maintained at 65°-70° by occasional cooling
5. customAfter the exothermic reaction
6. filtrationinorganic material is filtered off
7. washwashed three times with a little acetic acid
8. additionThe total filtrate is added dropwise
9. stirringwhile stirring well, to 11/2 l of water
10. stirringafter stirring for 2 hours
11. filtrationthe resulting precipitate is filtered off
12. washwashed neutral with water
13. customAfter drying in vacuo at 60°