反应详情

To a solution of 4-[(3-benzoyloxy-4-fluorobenzyl)(4-cyanophenyl)amino]-4H-[1,2,4]triazole (0.958 g, 2.32 mmol) in MeOH (10 mL) was added NaOH (0.25 g, 6.25 mmol), and the solution heated to reflux for 5 minutes and then concentrated in vacuo. Water (10 mL) was added and the milky suspension was neutralised (pH 7-8) with 2N HCl. The white precipitate was filtered off, washed with a small amount of water (5 mL) and dried under high vacuum to give STX488 as a white solid (0.476 g, 66%); δH (400 MHz, DMSO-d6) 4.95 (s, 2H), 6.70 (ddd, J=11.4, 8.4, 2.4, 1H), 6.75 (AA′BB′, 2H), 6.84 (dd, J=8.4, 2.4, 1H), 7.06 (dd, J=11.3, 8.4, 1H), 7.76 (AA′BB′, 2H), 8.75 (s, 2H), 9.90 (s, 1H—exchanges with D2O); LRMS (FAB+) m/z (rel. intensity) 310.1 (100, [M+H]+).

1. temperaturethe solution heated
2. temperatureto reflux for 5 minutes
3. concentrationconcentrated in vacuo
4. additionWater (10 mL) was added
5. filtrationThe white precipitate was filtered off
6. washwashed with a small amount of water (5 mL)
7. customdried under high vacuum