HRID1270402

反应详情

EQUATION

反应方程式

HRID 1270402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat reflux
  2. concentrationthe reaction was concentrated
  3. dissolutionredissolved in ethanol (10 mL)
  4. additionThe mixture was treated with concentrated H2SO4 (0.5 mL)
  5. temperatureheated
  6. temperatureat reflux
  7. waitAfter 1 h
  8. customthe cooled reaction mixture
  9. customwas partitioned between saturated aqueous NaHCO3 and CH2Cl2
  10. dry with materialThe organic layer was dried over sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated