HRID1189504
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 4-[1-(4-pentafluoroethyloxy-phenyl)-1H-[1,2,4]triazol-3-yl]-benzaldehyde (1.7 g, 4.4 mmol), sodium bromate (2.1 g, 13.9 mmol) and sodium bisulfate (0.53 g, 4.5 mmol) in acetonitrile (50 mL) was heated to reflux for 5 h, during which time a voluminous precipitate formed. The solution was then cooled and poured into water (100 mL), filtered, and dried to furnish the acid (1.67 g) as a white solid: mp 225° C.; 1H NMR (300 MHz, CDCl3) δ 10.1 (s, 1H), 8.63 (s, 1H), 8.35 (d, J=8.4 Hz, 2H), 8.5 (d, J=8.4 Hz, 2H), 7.85 (d, J=9 Hz, 2H), 7.43 (d, J=9 Hz, 2H); ESIMS m/z 399.2 (M+H+).
WORKUP
后处理
- temperatureto reflux for 5 h, during which time a voluminous precipitate
- customformed
- temperatureThe solution was then cooled
- filtrationfiltered
- customdried