HRID29525
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
5-phenyl-2-H-tetrazole (4 g, 27.36 mmol) was taken into NaOH (2.18 g, 54 mmol, dissolved in 10 ml of water), cooled to 0° C., methyl iodide (8.5 g, 60 mmol, dissolved in 40 ml acetone) was added and the reaction mixture was refluxed at 55° C. for 2 hours. The solvent was evaporated and the residue was dissolved in benzene. The benzene layer was washed with water, brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography using 60-120 mesh size silica gel (10% ethyl acetate in pet-ether as eluent) to obtain 2-methyl-5-phenyl-2H-tetrazole as white solid (2 g, 46%).
WORKUP
后处理
- temperaturethe reaction mixture was refluxed at 55° C. for 2 hours
- customThe solvent was evaporated
- dissolutionthe residue was dissolved in benzene
- washThe benzene layer was washed with water, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
- customThe residue was purified by column chromatography