HRID1061876
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
Methyl 1-methyl-6-[(1-trityl-1H-imidazol-4-yl)carbonyl]-2-naphthoate (20.7 g) was suspended in carbon tetrachloride (400 mL) and N-bromosuccinimide (7.5 g) and 2,2′-azobisisobutyronitrile (0.58 g) were added. The reaction mixture was heated under reflux for 5 hrs. and concentrated. The residue was diluted with saturated aqueous sodium hydrogen carbonate and extracted twice with ethyl acetate. The organic layers were combined, washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated to give a crude title compound (25.7 g) as a brown amorphous solid.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 5 hrs
- concentrationand concentrated
- additionThe residue was diluted with saturated aqueous sodium hydrogen carbonate
- extractionextracted twice with ethyl acetate
- washwashed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated