反应详情

温度

10 °C

A mixture of 0.244 mol of 1-benzhydryl-3-phthalimidoazetidine in 1000 ml of anhydrous methanol is heated at reflux for 15 minutes, then, after removing the heating bath, 0.339 mol of 85% hydrazine hydrate are added thereto. The mixture is heated at reflux for 30 minutes, then a solid white product begins to precipitate from the limpid solution thus obtained. The mixture is again heated for 90 minutes, then it is cooled at 10° C. One liter of diethyl ether is added to the mixture which is then filtered. After washing with ether, the solid product (35 g) is discarded and the mother-liquor is concentrated under reduced pressure. The residue is taken up with 500 ml of water and the pH of the solution is adjusted to 11 with sodium hydroxide. After extraction with 1 liter of diethyl ether, the ethereal phase is washed with water, dried on anhydrous sodium sulfate and evaporated under reduced pressure. Thus, the 3-amino-1-benzhydrylazetidine is obtained in the form of an oil which tends to solidify Yield 96.3%. By reaction with hydrochloric acid in a ispropanol/acetone mixture, the 3-amino-1-benzhydrylazetidine dihydrochloride is obtained which, after crystallization from isopropanol, melts at 108°-110° C.

1. temperatureis heated
2. temperatureat reflux for 15 minutes
3. additionare added
4. temperatureThe mixture is heated
5. temperatureat reflux for 30 minutes
6. customto precipitate from the limpid solution
7. customthus obtained
8. temperatureThe mixture is again heated for 90 minutes
9. filtrationis then filtered
10. washAfter washing with ether
11. concentrationthe mother-liquor is concentrated under reduced pressure
12. extractionAfter extraction with 1 liter of diethyl ether
13. washthe ethereal phase is washed with water
14. dry with materialdried on anhydrous sodium sulfate
15. customevaporated under reduced pressure