反应详情

To a solution of 4-piperidone monohydrate, hydrochloride (30.7 g; 0.2 mol), sodium carbonate (42 g; 0.4 mol) in water (160 mL) was added dichloromethane (500 mL). The mixture was stirred at room temperature and a solution of methyl malonylchloride (26 ml; 1.2 eq) in dichloromethane (100 mL) was added dropwise at room temperature, keeping the temperature of the reaction mixture below 30° C. The pH was maintained at 8 at the end of the addition. The mixture was stirred 4 hours at room temperature. The residue was extracted twice with dichloromethane, dried over magnesium sulfate and evaporate to yield the title compound (37.4 g).

1. customthe temperature of the reaction mixture below 30° C
2. temperatureThe pH was maintained at 8 at the end of the addition
3. stirringThe mixture was stirred 4 hours at room temperature
4. extractionThe residue was extracted twice with dichloromethane
5. dry with materialdried over magnesium sulfate
6. customevaporate