反应详情

Mercury(II) chloride (23 mg, 0.084 mmol) was added to a solution of N-[(3R,6S)-6-(2,3-difluorophenyl)-2-thioxo-1-(2,2,2-trifluoroethyl)azepan-3-yl]-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxamide (32 mg, 0.055 mmol) and methylamine (2.0 M in tetrahydrofuran; 274 μL, 0.547 mmol) in ethanol (1 mL). After 2 h, the mixture was filtered and concentrated. Purification by reverse phase HPLC(C-18, 95% water/acetonitrile→100% acetonitrile with 0.1% trifluoroacetic acid) gave the title compound as a bis trifluoroacetate salt (33 mg). MS 580.2415 (M+1).

1. filtrationthe mixture was filtered
2. concentrationconcentrated
3. customPurification by reverse phase HPLC(C-18, 95% water/acetonitrile→100% acetonitrile with 0.1% trifluoroacetic acid)