反应详情

Et3N (104 μL), HOBT (57 mg) and WSC hydrochloride (71 mg) were added to a DMF (4 mL) solution of 3,5-diethoxy-4-isoxazol-4-yl-benzoic acid (86 mg) and 6-(tetrazol-5-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (119 mg), and stirred overnight at room temperature. Water was added to the reaction liquid, the formed solid was taken out through filtration, and washed with water and ether. The resulting solid was purified through high-performance preparative liquid chromatography (0.1% TFA, water/acetonitrile) to obtain the title compound. 1H-NMR (400 MHz, DMSO-d6) δ: 9.18 (1H, s), 8.96 (1H, s), 8.42 (1H, d, J=4.0 Hz), 8.21 (1H, dd, J=8.0, 4.0 Hz), 7.33 (1H, d, J=8.0 Hz), 6.74 (2H, s), 4.32-4.18 (1H, m), 4.08 (4H, q, J=8.0 Hz), 3.64-3.20 (3H, m), 2.97 (2H, s), 2.10-1.75 (4H, m), 1.37 (6H, t, J=8.0 Hz). MS [M+H]+=545.

1. filtrationthe formed solid was taken out through filtration
2. washwashed with water and ether
3. customThe resulting solid was purified through high-performance preparative liquid chromatography (0.1% TFA, water/acetonitrile)