HRID2183624

反应详情

EQUATION

反应方程式

HRID 2183624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-acetylbenzo[b]thiophen-4-yl benzoate (0.13 g), potassium carbonate (0.18 g), tetrahydrofuran (25 ml) and 5M aqueous sodium hydroxide solution (10 ml) was heated under reflux for 1 hour, then cooled to ambient temperature and concentrated in vacuo. The aqueous residue was acidified by the addition of 5M hydrochloric acid (20 ml), then the product was extracted into dichloromethane (2×25 ml). The combined extracts were washed with water (20 ml), 10% aqueous sodium hydrogencarbonate solution (3×20 ml) and water (2×20 ml), then dried (MgSO4) and the solvent was removed in vacuo to give 1-(5-hydroxybenzo[b]thiophen-2-yl]ethan-1-one (0.07 g) as a yellow solid which was used without further purification.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. concentrationconcentrated in vacuo
  4. additionThe aqueous residue was acidified by the addition of 5M hydrochloric acid (20 ml)
  5. extractionthe product was extracted into dichloromethane (2×25 ml)
  6. washThe combined extracts were washed with water (20 ml), 10% aqueous sodium hydrogencarbonate solution (3×20 ml) and water (2×20 ml)
  7. dry with materialdried (MgSO4)
  8. customthe solvent was removed in vacuo