Sodium Iodide → 2-Benzyl-2h-1,2,3-triazole

1,2,3-Triazole (1523 mg, 22.05 mmol), sodium iodide (2203 mg, 14.7 mmol) and sodium hydroxide (882 mg, 22.05 mmol) were added to t-amyl alcohol (5.8 ml), and the mixture was refluxed under stirring for 1 hour. Benzyl chloride (1861 mg, 14.7 mmol) was dissolved in t-amyl alcohol (5.8 ml) and added dropwise under reflux over 1 hour. The mixture was refluxed under stirring for 1 hour. The mixture was cooled to room temperature and toluene (50 ml) was added. The mixture was washed with water (50×2), dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=3/1→1/3) to give 1-benzyl-1H-1,2,3-triazole (2.10 g) as white crystals, yield 90%, and 2-benzyl-2H-1,2,3-triazole (140 mg) as white crystals (yield 6%). 1-benzyl-1H-1,2,3-triazole

1. temperaturethe mixture was refluxed
2. additionadded dropwise
3. temperatureunder reflux over 1 hour
4. temperatureThe mixture was refluxed
5. stirringunder stirring for 1 hour
6. washThe mixture was washed with water (50×2)
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=3/1→1/3)

ORDレコード

ord-0ce0019280cb4a238e5e3f72338e79a9

出典データセット

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06743924B2