反应详情

温度

5 °C

A solution of 2-(2-(4-chloro-3-methoxyphenyl)-2-methylpropanoyl)-N-(4-fluorophenyl)-hydrazine carbothioamide (8.13 g, 0.02 mol) in 3N NaOH (270 mL) was heated at reflux 4 h with mechanical stirring. The reaction mixture was cooled to 5° C. and acidified with 5N HCl to pH=4. The resulting whited solids were collected by filtration, washed with diethyl ether and dried to give 5-(2-(4-chloro-3-methoxyphenyl)propan-2-yl)-4-(4-fluorophenyl)-4H-1,2,4-triazole-3-thiol (7.5 g, 96%). 1H NMR (400 MHz, DMSO-d6) δ 7.23-7.21 (d, 1H), 6.95-6.91 (t, 2H), 6.54 (d, 1H), 6.52-6.49 (dd, 1H), 6.45-6.41 (m, 2H), 3.67 (s, 3H), 1.45 (s, 6H).

1. temperatureat reflux 4 h with mechanical stirring
2. filtrationThe resulting whited solids were collected by filtration
3. washwashed with diethyl ether
4. customdried