반응 #352587

반응 방정식

4,5-diphenyltriazole

1,8-dibromooctane

potassium carbonate

→

2-(8-bromooctyl)-4,5-diphenyl-triazole

수율 54.3%

용매

butanone

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux temperature for 24 hours
3. 3
   여과The mixture was filtered
4. 4
   기타the solvent evaporated
5. 5
   기타to give an oily residue
6. 6
   workup.DISTILLATIONDistillation
7. 7
   기타to remove 1,8-dibromooctane and column chromatography on silica gel
8. 8
   세척eluted with a hexane

실험 절차

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

출처