反应详情

温度

50 °C

DMF (10 mL) and Et3N (1 mL) were added to 3-phenyl-1-pyridin-2-yl-1H-thieno[2,3-c]pyrazole-5-carboxylic acid (160 mg), 6-tetrazol-5-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (190 mg), EDCI (120 mg) and HOBT (90 mg), heated at 50° C. and stirred overnight. This was further stirred at 110° C. for 1 hour, then restored to room temperature, diluted with water, and its pH was adjusted at 1.5 with 1 N HCl added thereto. The formed crystal was taken out through filtration, washed with water, n-hexane and water, and dried in vacuum at 60° C. to obtain the title compound as a pale brown power. 1H-NMR (400 MHz, DMSO-d6) δ: 8.62-8.57 (1H, m), 8.44 (1H, d, J=2.2 Hz), 8.26 (1H, dd, J=8.0, 2.2 Hz), 8.16-8.06 (4H, m), 7.92 (1H, s), 7.55 (2H, t, J=8.0 Hz), 7.50-7.45 (1H, m), 7.41-7.34 (2H, m), 4.30-4.20 (2H, br m), 3.53 (2H, s), 3.01 (2H, s), 2.12-2.04 (2H, br m), 1.95-1.84 (2H, br m). MS [M+H]+=589.

1. stirringThis was further stirred at 110° C. for 1 hour
2. customrestored to room temperature
3. additionadded
4. filtrationThe formed crystal was taken out through filtration
5. washwashed with water, n-hexane and water
6. customdried in vacuum at 60° C.