反应详情

2-[(4-{[3-chloro-4-(pyridin-2-ylmethoxy)phenyl]amino}-1H-pyrazolo[3,4-d]pyrimidin-3-yl)oxy]ethanol (prepared as described in Example 4/50 mg, 0.12 mmol), hydantoin (36 mg, 0.36 mmol) and triphenylphosphine (94 mg) were dissolved in a 1:1 mixture of THF and DMF (1.2 ml). Ditertbutyl azodicarboxylate (69 mg, 0.3 mmol) was added at 0° C. and mixture was stirred at room temperature for 3 hours. After evaporation, the crude mixture was purified by preparative HPLC (column beta-basic, Hypercil 5 μm, 21×100 mm) eluting with a mixture of water and acetonitrile containing 2g/l of ammonium carbonate (gradient) to give the title compound (15 mg, 25%); NMR Spectrum: 3.88 (t, 2H), 3.96 (s, 2H), 4.37 (t, 2H), 5.29 (s, 2H), 7.24 (d, 1H), 7.36-7.38 (m, 1H), 7.58 (d, 1H), 7.78 (dd, 1H), 7.88 (t, 1H), 8.09 (s, 1H), 8.17 (s, 1H), 8.21 (s, 1H), 8.34 (s, 1H), 8.59 (d, 1H); Mass Spectrum: 495 (MH+).

1. customAfter evaporation
2. customthe crude mixture was purified by preparative HPLC (column beta-basic, Hypercil 5 μm, 21×100 mm)
3. washeluting with a mixture of water and acetonitrile containing 2g/l of ammonium carbonate (gradient)