HRID1061876

反应详情

EQUATION

反应方程式

HRID 1061876 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 5 hrs
  3. concentrationand concentrated
  4. additionThe residue was diluted with saturated aqueous sodium hydrogen carbonate
  5. extractionextracted twice with ethyl acetate
  6. washwashed with saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated