反应详情

With stirring, trifluoroacetic acid (10 ml) was added to 4-[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2yl]carbonyl-1-piperidinecarboxylic acid, 1,1-dimethylethyl ester (1.65 g, 3.77×10-3 mole). After 30 minutes the reaction was cooled in an ice bath and ether (150 ml) was added. The flask was stoppered and placed in the refrigerator. After several hours, the solid was collected by filtration, washed with EtzO, and dried by suction. Crystallization from ethanol/ether afforded [1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]-4-piperidinylmethanone, mono (trifluoroacetate) as colorless needles: 1.45 g (84%), m.p. 213°-215° C. (decomp).

1. temperatureAfter 30 minutes the reaction was cooled in an ice bath
2. waitAfter several hours
3. filtrationthe solid was collected by filtration
4. washwashed with EtzO
5. customdried by suction
6. customCrystallization from ethanol/ether