HRID584749
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
CONDITIONS
反应条件
- 温度
- 45 °C
PROCEDURE
实验过程
Dimethylcarbamic chloride was added to a mixture of 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-ol (200 mg, 0.673 mmol) and pyridine (0.114 ml, 1.41 mmol) in dichloromethane (5 ml). Then the solution was stirred at 45° C. for 17 hours. Water and ethyl acetate were poured into the mixture and the organic layer was separated, washed with water and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography (hexane-ethyl acetate 1:2). The desired product was washed with isopropyl ether to give 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-yl dimethylcarbamate. (88 mg, 35.5% yield)
WORKUP
后处理
- customthe organic layer was separated
- washwashed with water and brine
- dry with materialdried over magnesium sulfate
- customThe solvent was removed under reduced pressure
- customThe residue was purified by column chromatography (hexane-ethyl acetate 1:2)
- washThe desired product was washed with isopropyl ether