反应详情

26.3 g (0.1 mole) of 5-cyano-10-nitro-5H-dibenz[b,f]azepine are suspended in a mixture of 265 ml of ethylene glycol monoethyl ether and 75 ml of concentrated hydrochloric acid. 40 g of iron powder are added in small portions at 40° in the course of 40 minutes and the temperature is maintained at 40° by external cooling. The mixture is stirred for a further 2 hours at room temperature, is then heated to 80°, the precipitated product dissolving again, and is filtered through a heated suction filter, which is subsequently washed with ethylene glycol monoethyl ether. The crystallisation which commences in the filtrate is completed by adding 200 ml of water. After cooling for one hour in an ice-bath, filtration is carried out followed by washing with a mixture of ethylene glycol monoethyl ether and water in a ratio of 1:1. 5-cyano-10-oxo-10,11-dihydro-5H-dibenz[b,f]azepine is obtained which is identified, by comparing the IR spectra, with material from Example 27.

1. temperaturethe temperature is maintained at 40° by external cooling
2. temperatureis then heated to 80°
3. dissolutionthe precipitated product dissolving again
4. filtrationis filtered through a heated suction
5. filtrationfilter
6. washwhich is subsequently washed with ethylene glycol monoethyl ether
7. customThe crystallisation which
8. additionby adding 200 ml of water
9. temperatureAfter cooling for one hour in an ice-bath
10. filtrationfiltration
11. washby washing with a mixture of ethylene glycol monoethyl ether and water in a ratio of 1:1