反应详情

A mixture of pyridine-2-carboxylic acid (2.7 g) and 4-(aminomethyl)-1-tert-butoxycarbonylpiperidine (5.0 g) in dry xylene (50 ml) was heated under reflux under a Dean and Stark water separator for six hours. The cooled solution was diluted with ethyl acetate (150 ml), washed with aqueous oxalic acid solution (2M; 2×100 ml) then aqueous sodium hydrogen carbonate soultion (5M; 2×100 ml) and dried over magnesium sulphate. The solvent was removed in vacuo to give N-[(1-tert-butoxycarbonyl-4-piperidyl)methyl]pyridine-2-carboxamide (2.53 g) as an oil.

1. temperaturewas heated
2. washwashed with aqueous oxalic acid solution (2M; 2×100 ml)
3. dry with materialaqueous sodium hydrogen carbonate soultion (5M; 2×100 ml) and dried over magnesium sulphate
4. customThe solvent was removed in vacuo