HRID730312
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
To a mixture of 4-(4-trifluoromethyl-phenyl)-pyridine (5.0 g, 22 mmol) and methyltrioxorhenium (VII) (Aldrich) (110 mg, 0.45 mmol) in a 100-mL, round-bottomed flask was added CH2Cl2 (10 mL). Hydrogen peroxide (5 mL, Aldrich) was added drop-wise, and the reaction was stirred at room temperature under N2 for 48 h. The mixture was partitioned between CH2Cl2 and brine, and the aqueous layer was extracted with CH2Cl2 (40 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated in vacuo to give the title compound as an off-white solid. MS (ESI, pos. ion) m/z: 240 (M+1).
WORKUP
后处理
- customThe mixture was partitioned between CH2Cl2 and brine
- extractionthe aqueous layer was extracted with CH2Cl2 (40 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo