反应详情

[2-(4-Methoxybenzyl)-2H-[1,2,4]triazol-3-yl]methanol (0.50 g, 2.28 mmol) was dissolved in dichloromethane (10 ml), then triethylamine (0.36 ml, 2.60 mmol) was added. With cooling with ice, methanesulfonyl chloride (0.20 ml, 2.58 mmol) was added, followed by stirring at room temperature for 2 hours. The reaction liquid was concentrated, ethyl acetate was added, followed by washing. After drying over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure, and the resulting residue was dissolved in tetrahydrofuran (25 ml), then aqueous methylamine solution (40%, 5 ml) was added. After stirring at room temperature for 3 days, the reaction liquid was concentrated. This was diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain a pale yellow oil (0.44 g, 83%).

1. additionwas added
2. customThe reaction liquid
3. concentrationwas concentrated
4. additionethyl acetate was added
5. washby washing
6. dry with materialAfter drying over anhydrous sodium sulfate
7. customthe solvent was evaporated away under reduced pressure
8. dissolutionthe resulting residue was dissolved in tetrahydrofuran (25 ml)
9. additionaqueous methylamine solution (40%, 5 ml) was added
10. stirringAfter stirring at room temperature for 3 days
11. customthe reaction liquid
12. concentrationwas concentrated
13. additionThis was diluted with ethyl acetate
14. washwashed with water
15. dry with materialdried over anhydrous sodium sulfate
16. customThe solvent was evaporated away under reduced pressure