HRID1073888
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
1.61 g of 2,2-dimethyl-4-(2-pyridyl)-2H-1-benzopyran were dissolved in 10 ml of dichloromethane at room temperature and 2.0 g of m-chloroperbenzoic acid were added. After 1 hour the mixture was washed with sodium bisulphite solution, sodium bicarbonate solution and water. The organic phase was dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using ethyl acetate/ethanol/formic acid (40:4:1) for the elution. The product was obtained as an oil which solidified upon trituration with diethyl ether. Recrystallization from toluene gave 0.034 g of 2-(2,2-dimethyl-2H-1-benzopyran-4-yl)pyridine N-oxide of melting point 148-150° C.
WORKUP
后处理
- washAfter 1 hour the mixture was washed with sodium bisulphite solution, sodium bicarbonate solution and water
- dry with materialThe organic phase was dried over sodium sulphate
- customevaporated
- customThe residue was chromatographed on silica gel
- washfor the elution
- customThe product was obtained as an oil which
- customRecrystallization from toluene