反应详情

The title compound was prepared following procedure described for example 4, step 1, but starting from Intermediate 6 (116.2 mg; 0.50 mmol) and Intermediate 2 (106.1 mg; 0.50 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 suspended in ACN, filtrated and washed with cHex dried under vacuo, affording the title compound. 1H NMR (DMSO-d6, 300 MHz) δ 8.35-8.30 (m, 1H), 8.17 (d, J=1.3 Hz, 1H), 8.08-8.01 (m, 2H), 7.95 (dd, J=11.0, 1.3 Hz, 1H), 7.46-7.42 (m, 2H), 7.35 (dd, J=3.2, 1.1 Hz, 1H), 3.93 (s, 3H), 2.24 (s, 3H), 2.01 (s, 3H). LC/MS (Method B): 409.1 (M+H)+. HPLC (Method A) Rt 6.06 min (Purity: 93.6%).

1. customThe title compound was prepared following procedure
2. filtrationThe reaction mixture was filtered through a SPE NH2 column (2 g)
3. washrinsed with ACN
4. washrinsed with ACN
5. customAfter evaporation of the solvents
6. filtrationfiltrated
7. washwashed with cHex
8. customdried under vacuo