HRID1247875
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
- 80 °C
PROCEDURE
实验过程
A mixture of 30 mg (0.75 mmol) of powdered sodium hydroxide, 87 mg (0.59 mmol) of 3-cyano-1-nitrobenzene, 155 mg (0.75 mmol) of 2,6-di-t-butylphenol, and 1.0 mL of dimethylsulfoxide was heated at 80° C. for 90 minutes and poured into 10 mL of 1N HCl, and the resulting aqueous mixture was extracted with three 10 mL portions of diethyl ether. The ether layers were combined, dried over magnesium sulfate, and concentrated. Purification of the residue by preparative thin layer chromatography and crystallization afforded 98 mg (47% yield) of 2,6-di-t-butyl-4-(2'-cyano-4'-nitrophenyl)phenol.
WORKUP
后处理
- extractionthe resulting aqueous mixture was extracted with three 10 mL portions of diethyl ether
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customPurification of the residue
- customby preparative thin layer chromatography and crystallization