反应详情

A suspension of 4-carbamoyl-1-(4-methoxyphenyl)-pyridinium chloride (22.0 g) in methanol (250 ml) was hydrogenated at ambient temperature and pressure in the presence of 10% palladium-on-carbon catalyst (1.0 g) for 2 days. Further catalyst (0.75 g) was added, and when no more hydrogen was taken up, the catalyst was removed by filtration. The filtrate was basified by the addition of an excess of triethylamine and the solvent removed in vacua. The residue was partitioned between water and a 19:1 mixture of chloroform and methanol. The solvent was removed in vacuo from the organic layer and the residue dried in vacuo over phosphorus pentoxide to give 1-(4-methoxyphenyl)piperidine-4-carboxamide as a white solid (10 g), m.p. 178°-181° C.

1. customwas hydrogenated at ambient temperature
2. customthe catalyst was removed by filtration
3. additionThe filtrate was basified by the addition of an excess of triethylamine
4. customthe solvent removed in vacua
5. customThe residue was partitioned between water
6. additiona 19:1 mixture of chloroform and methanol
7. customThe solvent was removed in vacuo from the organic layer
8. dry with materialthe residue dried in vacuo over phosphorus pentoxide