HRID546257

反应详情

EQUATION

反应方程式

HRID 546257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In a round bottom flask with a reflux condenser was placed 2-(2,3-dihydro-benzo[b]thiophen-5-yl)-1-morpholin-4-yl-ethanethione (1.85 g, 6.62 mmol) and to it was added acetic acid (7.7 mL), concentrated sulfuric acid (1.1 mL) and water (2 mL). The reaction mixture was then heated at 100° C. for 4 h. After this time the solution was added to water (40 mL) and extracted with ethyl acetate (3×50 mL). The organics were dried over sodium sulfate, filtered and concentrated in vacuo. Purified using reverse phase HPLC to afford (2,3-dihydro-benzo[b]thiophen-5-yl)-acetic acid (525 mg, 41%) as a white solid.

WORKUP

后处理

  1. customIn a round bottom flask with a reflux condenser was placed
  2. extractionextracted with ethyl acetate (3×50 mL)
  3. dry with materialThe organics were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurified