反应详情

温度

90 °C

To a solution of 4-(4′-trifluoromethylbiphenyl-2-carbonylamino)piperidine (1.03 g) obtained in Example 8b) in dimethylformamide (5 mL) were added potassium carbonate (276 mg) and bromoacetic acid ethyl ester (223 μL). The mixture was stirred overnight at ambient temperature of 90° C., and then concentrated in vacuo. The residue was distributed with water and chloroform, and the aqueous layer was further extracted with chloroform. The organic layers were combined, washed with saturated brine, dried over sodium sulfate, concentrated in vacuo and purified by column chromatography on silica gel with chloroform:methanol=30:1 to give the title compound (598 mg).

1. concentrationconcentrated in vacuo
2. extractionthe aqueous layer was further extracted with chloroform
3. washwashed with saturated brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. custompurified by column chromatography on silica gel with chloroform