反应详情

A solution of 20 parts of ethyl 3-methoxy-4-oxo-1-piperidinecarboxylate, 12 parts of (-)-α-methylbenzenemethanamine, 2 parts of a solution of thiophene in ethanol 4% and 200 parts of methanol was hydrogenated at normal pressure and at room temperature with 4 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated in vacuo. The residue was purified by HPLC using a mixture of hexane, trichloromethane and methanol (50:49.5:0.5 by volume) as eluent. The pure A-fractions were collected and the eluent was evaporated, yielding 15.62 parts (51%) of (-)-ethyl cis-3-methoxy-4-[(1-phenylethyl)-amino]-1-piperidinecarboxylate as a residue (intermediate 103).

1. filtrationthe catalyst was filtered off
2. customthe filtrate was evaporated in vacuo
3. customThe residue was purified by HPLC
4. additiona mixture of hexane, trichloromethane and methanol (50:49.5:0.5 by volume) as eluent
5. customThe pure A-fractions were collected
6. customthe eluent was evaporated