反应详情

To a solution of 1-cyclohexylmethyl-4-aminopiperidine (9.8 g; 0.05 moles) in methyl ethyl ketone (100 ml), a solution of 2-methoxy-4-acetamido-5chlorobenzoyl chloride (14.4 g, 0.055 moles) in methyl ethyl ketone (100 ml) was slowly added at a temperature between 0° and 5° C. The mixture was stirred at the same temperature for 1 hour followed by 4 hours at room temperature. The precipitated solid was filtered off, washed with methyl ethyl ketone and recrystallized from a mixture of ethanol-water to give N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-acetamido-5-chlorobenzamide hydrochloride monohydrate (21 g), m.p. 219°-221° C.

1. waitfollowed by 4 hours at room temperature
2. filtrationThe precipitated solid was filtered off
3. washwashed with methyl ethyl ketone
4. customrecrystallized from a mixture of ethanol-water