反应详情

温度

90 °C

6-[(1-Methyl-1H-pyrazol-5-yl)amino]spiro[chroman-2,4′-piperidin]-4-one hydrochloride (46 mg), 1-hydroxybenzotriazole monohydrate (17 mg), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (27 mg), triethylamine (34 μL) and water (660 μL) were added in that order to a DMF (2 mL) solution of 3-(pyrrolidin-1-yl)-5-(tetrazol-5-yl)benzoic acid (27 mg), and stirred at 90° C. for 2 hours and 30 minutes. Water was added to the reaction liquid, and the formed precipitate was taken out through filtration, once dried, then washed with hexane/ethyl acetate=3/2, and taken out through filtration. After dried, the title compound was obtained as a yellow solid. 1H-NMR (400 MHz, DMSO-d6) δ: 7.92 (1.0H, s), 7.32 (1.0H, d, J=2.0 Hz), 7.21 (2.0H, s), 7.18-7.13 (2.0H, m), 6.99 (1.0H, d, J=9.2 Hz), 6.67 (1.0H, s), 5.89 (1.0H, s), 4.30-4.22 (1.0H, m), 3.61 (3.0H, s), 3.65-3.20 (3.0H, m), 2.81 (2.0H, s), 2.05-1.85 (9.0H, m), 1.85-1.70 (3.0H, m). MS [M+H]+=554.

1. filtrationthe formed precipitate was taken out through filtration
2. customonce dried
3. washwashed with hexane/ethyl acetate=3/2
4. filtrationtaken out through filtration
5. customAfter dried