反应详情

The title compound was prepared following procedure described for example 4, step 1, but starting from Intermediate 36 and Intermediate 51. The reaction mixture was filtered through a SPE NH2 column (10 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), affording the title compound as a pale yellow oil. 1H NMR (CDCl3) δ 8.43 (d, J=1.3 Hz, 1H), 8.19-8.16 (m, 2H), 8.11 (d, J=7.5 Hz, 1H), 7.61-7.47 (m, 2H), 7.41-7.34 (m, 3H), 7.29-7.23 (m, 1H), 7.13-7.10 (m, 1H), 4.27-4.18 (m, 2H), 3.80 (s, 2H), 3.33 (s, 3H), 3.24 (s, 2H), 2.48-2.29 (m, 5H), 1.50 (s, 9H), 1.05 (t, J=7.6 Hz, 3H). LC/MS (Method B): 528.3 (M+H)+. HPLC (Method A) Rt 5.05 min (Purity: 98.4%).

1. customThe title compound was prepared following procedure
2. filtrationThe reaction mixture was filtered through a SPE NH2 column (10 g)
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)