反应详情

To a warm solution of N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-acetamido-5-chlorobenzamide (10 g; 0.023 moles) in diethyl ether (300 ml) a solution of methyl iodide (1.8 ml; 0.033 moles) in diethyl ether (25 ml) was added. The mixture was stirred at room temperature for 1 hour and then heated under reflux for 2 hours. An additional amount of methyl iodide (1 g; 0.0023 moles) was added and the reflux of the mixture was kept up for 3 more hours. The mixture was then evaporated in vacuo and the residue recrystallized from a mixture of diethyl ether-ethanol. N-(1-Cyclohexylmethylpiperid-4-yl)-2-methoxy-4-acetamido-5-chlorobenzamide methyl iodide (10.5 g), m.p. 209°-211° C., was thus obtained.

1. temperatureheated
2. temperatureunder reflux for 2 hours
3. temperaturethe reflux of the mixture
4. customThe mixture was then evaporated in vacuo
5. customthe residue recrystallized from a mixture of diethyl ether-ethanol