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 solution of N-(pyridin-2-yl)-2-(2-(trifluoromethyl)phenyl)-1H-benzo[d]imidazole-4-carboxamide (10; 100 mg, 0.26 mmol) in CH2Cl2 (10 mL) was added mCPBA (140 mg, 0.81 mmol) under nitrogen. The mixture was stirred at room temperature for 12 h. A saturated aqueous solution of K2CO3 (10 mL) was added and the mixture was extracted with CH2Cl2 (3×10 mL). The combined organic layers were dried (Na2SO4), concentrated under reduced pressure. The resulting residue was purified by chromatography (CH2Cl2:methanol=20:1) to give 2-(2-(2-(trifluoromethyl)phenyl)-1H-benzo[d]imidazole-4-carboxamido)pyridine 1-oxide (Compound 329) (60.0 mg, 58%) as a colorless solid. MS (ESI) calcd for C20H13F3N4O2: 398.10; found: 399 [M+H].
WORKUP
后处理
- extractionthe mixture was extracted with CH2Cl2 (3×10 mL)
- dry with materialThe combined organic layers were dried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customThe resulting residue was purified by chromatography (CH2Cl2:methanol=20:1)