反应详情

温度

70 °C

To a solution of 16.3 g of the N-[3-[3-(piperidinomethyl)phenoxy]propyl]phthalimide in 150 ml of methanol was added 2.3 g of hydrazine monohydrate, and the mixture was heated at 70° C. for 4 hours. The mixture was cooled, then the solvent was distilled off, 30 ml of 6N hydrochloric acid was added to the residue, and the mixture was heated at 60° C. for 15 minutes. The resulting mixture was cooled, the insolubles were then filtered off, the solution was made alkaline with potassium hydroxide and subjected to extraction with a mixture of ethyl acetate and diethyl ether (1:1), and the organic layer was dried over magnesium sulfate and thereafter distilled to remove the solvent, giving 8.3 g of pale yellow oily 3-[3-(1-piperidinomethyl)phenoxy]propylamine (yield 78% ).

1. temperatureThe mixture was cooled
2. distillationthe solvent was distilled off
3. addition30 ml of 6N hydrochloric acid was added to the residue
4. temperaturethe mixture was heated at 60° C. for 15 minutes
5. temperatureThe resulting mixture was cooled
6. filtrationthe insolubles were then filtered off
7. extractionsubjected to extraction with a mixture of ethyl acetate and diethyl ether (1:1)
8. dry with materialthe organic layer was dried over magnesium sulfate
9. distillationdistilled
10. customto remove the solvent