反应详情

In 20 ml of toluene, were added 1.0 g of the compound obtained in Example 11 and 500 mg of 4-aminomethylpiperidine. The resulting mixture was refluxed using a Dean-Stark device under heating for 2 hours to remove the produced water. The solvent was then evaporated, and 20 ml of anhydrous methanol was added to dissolve the residue. To the obtained solution, was added 100 mg of 5% palladium-carbon. The mixture was stirred at room temperature under hydrogen atmosphere. After 4 hours, 200 mg of the 5% palladium-carbon was further added, and the reaction mixture was stirred for another 65 hours. The catalyst was separated by filtration, and the reaction mixture was concentrated. The resulting concentrate was then dissolved in a mixed solvent of water-dichloromethane, and the aqueous layer was separated and concentrated to afford 0.82 g (60%) of the title compound as a light-yellow oily substance.

1. temperatureThe resulting mixture was refluxed
2. temperatureunder heating for 2 hours
3. customto remove the produced water
4. customThe solvent was then evaporated
5. addition20 ml of anhydrous methanol was added
6. dissolutionto dissolve the residue
7. additionTo the obtained solution, was added 100 mg of 5% palladium-carbon
8. addition200 mg of the 5% palladium-carbon was further added
9. stirringthe reaction mixture was stirred for another 65 hours
10. customThe catalyst was separated by filtration
11. concentrationthe reaction mixture was concentrated
12. concentrationThe resulting concentrate
13. dissolutionwas then dissolved in a mixed solvent of water-dichloromethane
14. customthe aqueous layer was separated
15. concentrationconcentrated