反应详情

A mixture of methyl 2-bromo-2-methylpropanoate (80.87 ml, 5 equiv), 4-piperidone hydrochloride monohydrate (19.6 g, 1 equiv), acetonitrile (200 ml) and potassium carbonate (69.1 g, 4 equiv) was heated at reflux under nitrogen with mechanical stirring for 17.5 h then cooled in an ice bath before adding diethyl ether (100 ml). Filtration through celite followed by flash chromatography (silica, 10-50% ethyl acetate in hexane) and evaporation of the product fractions gave the desired product as a yellow oil (14.28 g).

1. temperaturewas heated
2. temperatureat reflux under nitrogen
3. temperaturethen cooled in an ice bath
4. filtrationFiltration through celite
5. customfollowed by flash chromatography (silica, 10-50% ethyl acetate in hexane) and evaporation of the product fractions