反应详情

Title compound was prepared following general procedure 2 starting from Intermediate 14 (308 mg; 1.2 mmol) and Intermediate 3 (228 mg; 1.2 mmol). The reaction mixture was diluted with Et2O, washed with water and brine and evaporated under vacuum. Purification by silica column chromatography (EtOAc/c-Hex, 30/70 to 70/30) afforded the title compound as a pink powder. 1H NMR (DMSO-d6) δ 12.92 (br s, 0.5H), 12.71 (br s, 0.5H), 8.38 (d, J=6.0 Hz, 1H), 8.34 (d, J=1.3 Hz, 1H), 8.26-8.12 (m, 2H), 7.80 (d, J=6.8 Hz, 1H), 7.43 (d, J=8.1 Hz, 1H), 7.39-7.25 (m, 3H), 7.16 (d, J=7.0 Hz, 1H), 4.27-4.14 (m, 2H), 3.26 (s, 3H), 2.65 (s, 1.5H), 2.62 (s, 1.5H), 2.05 (s, 3H). LC/MS (method B): 409.3 (M−H)−; 411.3 (M+H)+. HPLC (Method A) Rt 4.11 min (Purity: 100.0%).

1. customTitle compound was prepared
2. washwashed with water and brine
3. customevaporated under vacuum
4. customPurification by silica column chromatography (EtOAc/c-Hex, 30/70 to 70/30)