反应详情

To a solution of 2-(2-isopropyl-2H-[1,2,4]triazol-3-yl)-8-piperidin-4-yl-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene 375 TFA salt (300 mg, 0.59 mmol) in THF (5 mL) was added potassium carbonate (285 mg, 2.10 mmol) followed by 2-bromo-N-methylacetamide (99 mg, 0.65 mmol). The reaction mixture was stirred for 3 hours before being diluted with DCM and water. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo. The resulting residue was triturated with diethyl ether to give 508 as a brown solid (226 mg, 82%). LCMS: RT=3.21 min, [M+H]+=467. 1H NMR δ (ppm) (DMSO-d6): 8.28 (1H, d, J=8.19 Hz), 8.10 (1H, s), 7.75-7.68 (1H, m), 7.10 (1H, dd, J=8.24, 1.81 Hz), 6.96 (1H, d, J=1.76 Hz), 5.86-5.77 (1H, m), 4.36 (2H, t, J=5.02 Hz), 3.42 (2H, t, J=5.03 Hz), 2.91-2.87 (4H, m), 2.64 (3H, d, J=4.74 Hz), 2.55-2.45 (1H, m), 2.19-2.17 (2H, m), 1.76-1.75 (4H, m), 1.55 (6H, d, J=6.59 Hz)

1. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
2. concentrationconcentrated in vacuo
3. customThe resulting residue was triturated with diethyl ether