HRID2070923
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
A solution of 4-isopropylpyridine and 1.5 mL of 30% H2O2 in 7 mL of AcOH was heated at 135° C. A total of 15.4 mL of H2O2 was added in 4 portions, and the solution was refluxed for 2 h. Chloroform and water were added, the layers were separated, and the aqueous layer was extracted 3 times with CHCl3. The combined extracts were dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (5% MeOH/CHCl3) provided 139 mg of the 4-isopropylpyridine N-oxide as an orange oil.
WORKUP
后处理
- temperaturethe solution was refluxed for 2 h
- customthe layers were separated
- extractionthe aqueous layer was extracted 3 times with CHCl3
- dry with materialThe combined extracts were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customPurification by flash silica gel chromatography (5% MeOH/CHCl3)