HRID419719
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
Add dimethyl sulfoxide (0.3 M, 2.7 mL) to powdered potassium hydroxide (1.5 equiv, 1.217 mmoles; 68 mg). Add 1-Benzyl-4-[5-(3-chloro-4-fluoro-phenyl)-1H-imidazol-2-yl]-piperidine (300 mg, 1.00 equiv; 0.811 mmoles), dropwise add iodoethane (1.1 equiv, 0.892 mmoles; 71 μL) over 8 min. Stir the reaction for 60 minutes, then dilute with water (120 mL) plus saturated sodium chloride (25 mL) and extract four times with DCM. Wash the organic extracts with water, then saturated aqueous sodium chloride, and dry with MgSO4. Filter and purify on silica gel with 10% methanol/acetonitrile to give 262 mg (0.659 mmol, 81%) of 1-Benzyl-4-[4-(3-chloro-4-fluoro-phenyl)-1-ethyl-1H-imidazol-2-yl]-piperidine.
WORKUP
后处理
- customthe reaction for 60 minutes
- extractionextract four times with DCM
- washWash the organic extracts with water
- dry with materialsaturated aqueous sodium chloride, and dry with MgSO4
- filtrationFilter
- custompurify on silica gel with 10% methanol/acetonitrile