反应详情

10 mmole of 3-mercapto-1H-1,2,4-triazole was dissolved in 20 ml ethanol, then 10 mmole EtOK was added, and stirred for 5 minutes. 10 mmole of ((chloromethyl)phenylethyl)trimethoxysilane was added to the solution, and stirred for 6 hours. The white precipitate was removed by filtration, the solvent in the filtrate was removed in vacuum. The obtained solid was dissolved in methanol, and separated with a Si gel column (solvents: 7 ethylacetate/3 hexane in volume). Yield: 53%. 1H NMR (CDCl3) of Precursors 6: δ(ppm) 8.09 (1H, s), 7.19 (4H, m), 4.29 (2H, s), 3.55 (9H, s), 2.72 (2H, t, JH-H=8.50), 1.02 (2H, t, JH-H=8.50).

1. stirringstirred for 6 hours
2. customThe white precipitate was removed by filtration
3. customthe solvent in the filtrate was removed in vacuum
4. dissolutionThe obtained solid was dissolved in methanol
5. customseparated with a Si gel column (solvents: 7 ethylacetate/3 hexane in volume)