反应详情

To a mixture consisting of 1.5 g (7.5 mmol) of the ketone derivative, i.e., (3-propionyl-5-phenylisoxazole) prepared above in the procedure (3), 0.99 g (8.2 mmol) of piperidine hydrochloride, 0.36 g of paraformaldehyde and 3 ml of dioxane, 0.03 ml of 12N-hydrochloric acid was added. The resultant mixture was heated under reflux for 2 hours. After completion of the reaction, ethyl ether was added. Colorless crystals thus formed were collected by filtration and added to a saturated aqueous solution of sodium hydrogencarbonate. The solution was extracted with ethyl ether. The solvent was distilled off so that 3-(2-methyl-3-piperidinopropionyl) -5-phenylisoxazole was obtained as colorless crystals. Analytical results of the crystals obtained: Yield: 1.2 g (48.1%). Melting point: 87°-89° C.

1. additionwas added
2. temperatureunder reflux for 2 hours
3. additionwas added
4. customColorless crystals thus formed
5. filtrationwere collected by filtration
6. additionadded to a saturated aqueous solution of sodium hydrogencarbonate
7. extractionThe solution was extracted with ethyl ether
8. distillationThe solvent was distilled off so that 3-(2-methyl-3-piperidinopropionyl) -5-phenylisoxazole
9. customwas obtained as colorless crystals
10. customAnalytical results of the crystals
11. customobtained