HRID1376378
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 mixture of 4,5-diphenyltriazole (11 g), 1,8-dibromooctane (67.6 g), and potassium carbonate (10.31 g) in dry butanone (300 ml ) was heated at reflux temperature for 24 hours. The mixture was filtered and the solvent evaporated to give an oily residue. Distillation to remove 1,8-dibromooctane and column chromatography on silica gel eluted with a hexane:ethyl acetate gradient gave 2-(8-bromooctyl)-4,5-diphenyl-triazole (11.13 g, 54%) as an oil. NMR d (CDCl3) 1.2-1.5 (8H, m, 4×CH2), 1.84 (2H, m, CH2), 2.05 (2H, m, CH2), 3.37 (2H, t, Br-CH2), 4.47 (2H, t, N-CH2), 7.3- 7.6 (10H, m, 2×Ph) ppm
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux temperature for 24 hours
- filtrationThe mixture was filtered
- customthe solvent evaporated
- customto give an oily residue
- distillationDistillation
- customto remove 1,8-dibromooctane and column chromatography on silica gel
- washeluted with a hexane