HRID978115

反应详情

EQUATION

反应方程式

HRID 978115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 4-hydroxy-3-methylbenzofuran-2-carboxylate (220 mg, 1 mmol) in dichloroethane (10 ml) was added aluminum chloride (665 mg, 5 mmol). To the resulting brown solution was added acetyl chloride (0.178 ml, 2.5 mmol). The mixture was stirred for 5 hours at room temperature. Ice and water (20 ml) was added. The mixture was extracted with ethyl acetate. The extracts were dried and concentrated to a white solid which was then treated with 1 ml of 10% K2CO3 aqueous solution in 10 ml methanol for 2 hours. The resulting mixture was poured into 0.1N HCl (25 ml) and filtered. The solid obtained was recrystallized from ethyl acetate/toluene to give the title compound (130 mg, 50%).

WORKUP

后处理

  1. extractionThe mixture was extracted with ethyl acetate
  2. customThe extracts were dried
  3. concentrationconcentrated to a white solid which
  4. additionwas then treated with 1 ml of 10% K2CO3 aqueous solution in 10 ml methanol for 2 hours
  5. additionThe resulting mixture was poured into 0.1N HCl (25 ml)
  6. filtrationfiltered
  7. customThe solid obtained
  8. customwas recrystallized from ethyl acetate/toluene