HRID1270402
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Ethyl (3-acetyl-4-bromo-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl)acetate (500 mg, 1.47 mmol) was dissolved in ethanol (10 mL) and 6 M aqueous HCl (20 mL) and heated at reflux. After 2 h, the reaction was concentrated and redissolved in ethanol (10 mL). The mixture was treated with concentrated H2SO4 (0.5 mL) and heated at reflux. After 1 h, the cooled reaction mixture was partitioned between saturated aqueous NaHCO3 and CH2Cl2. The organic layer was dried over sodium sulfate, filtered, and concentrated to give the title compound. MS: m/z=301 (M+1).
WORKUP
后处理
- temperatureat reflux
- concentrationthe reaction was concentrated
- dissolutionredissolved in ethanol (10 mL)
- additionThe mixture was treated with concentrated H2SO4 (0.5 mL)
- temperatureheated
- temperatureat reflux
- waitAfter 1 h
- customthe cooled reaction mixture
- customwas partitioned between saturated aqueous NaHCO3 and CH2Cl2
- dry with materialThe organic layer was dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated