反应详情

Dissolve isonipecotic acid methyl ester in formaldehyde (19.4 mL of a 37.5% solution in water, 262 mmol) and treat with formic acid (10.2 mL of a 90% solution, 240 mmol). Heat on a steam bath for 2 hours and evaporate the solvent in vacuo. Dissolve the residue in ethyl ether, dry (MgSO4), filter and evaporate the filtrate in vacuo. Purify by distillation under an argon atmosphere to give 1-methyl-4-piperidinecarboxylic acid, methyl ester as a clear colorless oil (bp 195°-205° C., 760 mm).

1. temperatureHeat on a steam bath for 2 hours
2. customevaporate the solvent in vacuo
3. dissolutionDissolve the residue in ethyl ether
4. dry with materialdry (MgSO4)
5. filtrationfilter
6. customevaporate the filtrate in vacuo
7. distillationPurify by distillation under an argon atmosphere