反应详情

5-(3-Phthalimidopropyl)-5H-dibenzo[a,d]cycloheptene, 2.15 g. (0.0054 mole), is dissolved in 50 ml. of hot 95% ethanol. Hydrazine hydrate, 0.6 ml., is added and the solution heated to refluxing for 2 hours. The solution then is cooled, acidified, and the precipitate of phthalhydrazide removed by filtration. Ethanol is distilled from the filtrate under reduced pressure and the residue dissolved in 40 ml. of water. The filtered solution is evaporated by heating under reduced pressure to a volume of approximately 20 ml. Upon cooling, the hydrochloride salt of 5-(3-aminopropyl)-5H-dibenzo[a,d]cycloheptene is precipitated in a yield of 1.35 g. (87.5%). After recrystallization from a mixture of ethanol and ether and from isopropyl alcohol, an analytical sample melted at 263°-265° C., dec.

1. dissolution(0.0054 mole), is dissolved in 50 ml
2. addition, is added
3. temperaturethe solution heated
4. temperatureto refluxing for 2 hours
5. temperatureThe solution then is cooled
6. customthe precipitate of phthalhydrazide removed by filtration
7. distillationEthanol is distilled from the filtrate under reduced pressure
8. dissolutionthe residue dissolved in 40 ml
9. customThe filtered solution is evaporated
10. temperatureby heating under reduced pressure to a volume of approximately 20 ml
11. temperatureUpon cooling
12. customthe hydrochloride salt of 5-(3-aminopropyl)-5H-dibenzo[a,d]cycloheptene is precipitated in a yield of 1.35 g
13. customAfter recrystallization
14. additionfrom a mixture of ethanol and ether