反应详情

A solution of dichloromethane/trifluoroacetic acid (1/1) [1 mL] was added to (imino-{4-[2′-(4-methanesulfonyl-butyrylamino)-6′-methyl-biphenyl-3-sulfonyl]-5-methylsulfanyl-thiophen-2-yl}-methyl)-carbamic acid tert-butyl ester (0.011 g, 0.017 mmol) [example 209, step b] at room temperature and stirred for 1 hour. The reaction mixture was evaporated and purified via reverse-phase HPLC [acetonitrile/water (0.01% TFA)] to give the title compound (0.004 g, 36%) as a solid. 1H-NMR (MeOD): δ 8.29 (s, 1H), 8.04 (md, 1H, J=6.4 Hz), 7.87 (t, 1H, J=2.0 Hz), 7.69 (t, 1H, J=7.6 Hz), 7.54 (md, 1H, J=7.6 Hz), 7.34 (t, 1H, J=7.6 Hz), 7.28 (d, 1H, J=7.2 Hz), 7.18 (d, 1H J=7.2 Hz), 2.91 (s, 3H), 2.78 (t, 2H, J=7.6 Hz), 2.72 (s, 3H), 2.18 (t, 2H, J=7.6 Hz), 2.07 (s, 3H), 1.74 (m, 2H). ESI-MS (m/z): Calcd. for C24H27N3O5S4: 566.1; found: 566.8.

1. customThe reaction mixture was evaporated
2. custompurified via reverse-phase HPLC [acetonitrile/water (0.01% TFA)]