反应详情

1-[2-[3-(3,4-Dichloro-phenyl)-1-(3,4,5-trimethoxy-benzoyl)-pyrrolidin-3-yl]-ethyl]-4-phenyl-piperidine-4-carboxylic acid (0.2566 g, 0.4 mmol), N,N-dimethylethylenediamine (0.05 mL, 0.48 mmol), HOBt (65 mg, 0.48 mmol), EDC (92 mg, 0.48 mmol), DIEA (0.08 mL, 0.48 mmol) were combined in dichloromethane (20 mL). The mixture was stirred for 72 h at ambient temperature. The mixture was extracted with H2O. The organic phase was dried over MgSO4, filtered, and concentrated in vacuo to obtain a residue. The residue was chromatographed using a Vydac (25×250 mm) C-18 HPLC column to give the title compound: Rt =28 minutes (gradient elution with CH3CN/H2O(0.1% TFA; flow rate=1.0 ml/min.) 10% CH3CN for 10 minutes, 30% CH3CN for 15 minutes, 40% CH3 CN for 15 minutes, 50% CH3CN for 10 minutes, and then 100% CH3 CN).

1. extractionThe mixture was extracted with H2O
2. dry with materialThe organic phase was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto obtain a residue
6. customThe residue was chromatographed