反应详情

温度

80 °C

6-(Tetrazol-5-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (232 mg), 3-methyl-1-pyridin-2-yl-1H-thieno[2,3-c]pyrazole-5-carboxylic acid (155 mg), EDCI (153 mg) and HOBT (122 mg) were suspended in Et3N (1 mL) and DMF (8 mL). The suspension was stirred at 80° C. for 1.5 hours under heat, then cooled to room temperature, and chloroform (1.8 mL) was added thereto. Its pH was adjusted at 2.5 with 1 N HCl added thereto, and this was diluted with water, and Et2O was added thereto. The formed crystal was taken out through filtration, washed with water and Et2O—CHCl3, and dried in vacuum to obtain the title compound as a pale yellow powder. 1H-NMR (400 MHz, DMSO-d6): δ 8.53 (1H, d, J=4.4 Hz), 8.44 (1H, s), 8.25 (1H, d, J=8.5 Hz), 8.01 (1H, t, J=7.8 Hz), 7.90 (1H, d, J=8.5 Hz), 7.61 (1H, s), 7.37 (1H, d, J=8.8 Hz), 7.31 (1H, t, J=5.9 Hz), 6.44 (2H, s), 4.20 (2H, d, J=12.9 Hz), 3.48 (2H, br s), 2.52 (3H, s), 2.06 (2H, d, J=13.7 Hz), 1.94-1.81 (2H, m). MS [M+H]+=527.

1. temperatureunder heat
2. temperaturecooled to room temperature
3. additionadded
4. additionwas added
5. filtrationThe formed crystal was taken out through filtration
6. washwashed with water and Et2O—CHCl3
7. customdried in vacuum