反应详情

The title compound was prepared following procedure described for example 4, step 1, but starting from Intermediate 28 (230.67 mg; 0.90 mmol) and Intermediate 55 (184.97 mg; 0.75 mmol). The reaction mixture was filtered through a SPE NH2 column (2 g) and rinsed with ACN. The filtrate was passed through a SPE SCX column (2 g) and rinsed with ACN. After evaporation of the solvents, the crude product was purified by flash chromatography (c-hex/(DCM/EtOAc 1:1) gradient from 1:0 to 1:1). The white solid was washed with MeOH affording the title compound as a white powder. 1H NMR (CDCl3, 300 MHz) δ 8.44-8.43 (m, 1H), 8.35 (d, J=6.1 Hz, 1H), 8.18 (dd, J=7.9, 1.8 Hz, 1H), 7.77 (d, J=10.1 Hz, 1H), 7.35 (d, J=7.9 Hz, 1H), 7.32-7.24 (m, 3H), 7.13 (d, J=7.2 Hz, 1H), 4.27-4.18 (m, 2H), 3.99 (s, 3H), 3.34 (s, 3H), 2.08 (s, 3H). LC/MS (Method B): 467.1 (M+H)+. HPLC (Method A) Rt 6.09 min (Purity: 98.8%).

1. filtrationThe reaction mixture was filtered through a SPE NH2 column (2 g)
2. washrinsed with ACN
3. washrinsed with ACN
4. customAfter evaporation of the solvents
5. customthe crude product was purified by flash chromatography (c-hex/(DCM/EtOAc 1:1) gradient from 1:0 to 1:1)
6. washThe white solid was washed with MeOH affording the title compound as a white powder