反应详情

A solution of 4-(4-aminophenoxy)-1-methyl-4-phenylpiperidine (2.82 g, 10 mM), in THF (75 ml) was added over 2 hours to a refluxing solution of amyl nitrite (2.7 ml, 20 mM) in THF (30 ml). After 5 hours at reflux amyl nitrite (1.5 ml) was added and the mixture maintained at reflux for 24 hours. The solvent was removed under reduced pressure and the residue partitioned between 2 N hydrochloric acid (50 ml) and ether (50 ml). The aqueous phase was basified (pH9) and extracted with ether (2×100 ml). The organic phase was dried and the solvents removed under reduced pressure. Sublimation of the residue at 1.0 mbar pressure (bath temp. 100°) gave the title compound (700 mg), m.p. 103°-4°.

1. additionwas added
2. temperaturethe mixture maintained
3. temperatureat reflux for 24 hours
4. customThe solvent was removed under reduced pressure
5. customthe residue partitioned between 2 N hydrochloric acid (50 ml) and ether (50 ml)
6. extractionextracted with ether (2×100 ml)
7. customThe organic phase was dried
8. customthe solvents removed under reduced pressure