反应详情

温度

80 °C

A vial charged with tert-butyl 4-(2-(2-(N-(1,2,4-thiadiazol-5-yl)sulfamoyl)-1,2,3,4-tetrahydroisoquinolin-5-yl)-5-(trifluoromethyl)phenyl)-5,6-dihydropyridine-1(2H)-carboxylate (0.305 g, 0.491 mmol) was treated with HCl 4N in dioxane (3.07 ml, 12.26 mmol) then was heated to 80° C. for one hour. The reaction mixture was cooled to room temperature and was diluted with diethyl ether. The resulting white solid was filtered off and dried yielding 5-(2-(1,2,3,6-tetrahydropyridin-4-yl)-4-(trifluoromethyl)phenyl)-N-(1,2,4-thiadiazol-5-yl)-3,4-dihydroisoquinoline-2(1H)-sulfonamide hydrochloride (0.242 g, 0.434 mmol). [M+H]+=522.0. 1H NMR (400 MHz, DMSO-d6) δ ppm: 8.81 (br. s., 2H), 8.35-8.44 (m, 1H), 7.73 (d, J=8.0 Hz, 1H), 7.60 (d, J=1.3 Hz, 1H), 7.42 (d, J=7.8 Hz, 1H), 7.18-7.28 (m, 2H), 7.02 (d, J=6.6 Hz, 1H), 5.72 (br. s., 1H), 4.22-4.36 (m, 2H), 3.31-3.52 (m, 4H), 3.26 (m, 2H), 2.83-3.08 (m, 2H), 1.91-2.20 (m, 2H)

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationThe resulting white solid was filtered off
3. customdried