反应详情

75 g. (0.46 mol) β-4-phenylpiperidine is heated with 38 g. (0.46 mol) 2-chloroethanol for 5 hours at about 120° C. After cooling, the reaction mixture is dissolved in 500 ml. water, rendered alkaline with potassium carbonate, extracted with 1 liter ether, dried, evaporated and the residue distilled in a high vacuum. There is obtained 55 g. (61% of theory) β-(4-phenyl-piperidino)-ethanol (b.p. 155° C./0.2 mm.Hg.), which is dissolved in 500 ml. chloroform. The corresponding hydrochloride is then precipitated out by the addition of dry hydrogen chloride. 50 ml. thionyl chloride is added and the reaction mixture heated under reflux for 5 hours and cooled. The precipitated product is filtered off, dissolved in 300 ml. water and rendered alkaline with 10N aqueous sodium hydroxide solution. The precipitated base is extracted with 500 ml. ether, dried and evaporated. There is obtained 45 g. (75% of theory) β-(4-phenyl-piperidino)-ethyl chloride.

1. temperatureAfter cooling
2. dissolutionthe reaction mixture is dissolved in 500 ml
3. extractionextracted with 1 liter ether
4. customdried
5. customevaporated
6. distillationthe residue distilled in a high vacuum
7. customThere is obtained 55 g
8. customThe corresponding hydrochloride is then precipitated out by the addition of dry hydrogen chloride
9. additionthionyl chloride is added
10. temperaturethe reaction mixture heated
11. temperatureunder reflux for 5 hours
12. temperaturecooled
13. filtrationThe precipitated product is filtered off
14. dissolutiondissolved in 300 ml
15. extractionThe precipitated base is extracted with 500 ml
16. dry with materialether, dried
17. customevaporated
18. customThere is obtained 45 g