反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2.8 Milliliters of acetic anhydride was added to 15 ml of a pyridine solution containing 0.62 g of 4-[(4-nitrophenyl)amino]-4H-1,2,4-triazole at room temperature and the mixture was stirred for about 2 hours. After completion of reaction, the solvent was removed by distillation under reduced pressure, and a proper amount of an aqueous sodium hydrogencarbonate solution was added to the residue obtained, which was then extracted several times each with ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography to give 0.52 g of 4-[N-acetyl-N-(4-nitrophenyl)amino]-4H-1,2,4-triazole from the chloroform/methanol (100/1) eluate.
WORKUP
后处理
- customAfter completion of reaction
- customthe solvent was removed by distillation under reduced pressure
- additiona proper amount of an aqueous sodium hydrogencarbonate solution was added to the residue
- customobtained
- extractionwhich was then extracted several times each with ethyl acetate
- washThe ethyl acetate layer was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was removed by distillation under reduced pressure
- customThe residue was purified by silica gel column chromatography