HRID748951

反应详情

EQUATION

反应方程式

HRID 748951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 2,2-dimethyl-propionic acid 2,3-dibromo-benzo[b]thiophen-6-yl ester (32 g, 82 mmol) in ethanol (725 mL), add 50% aqueous solution of potassium hydroxide (39 mL, 328 mmol) and heat to reflux for 4 hours. Concentrate in vacuo to ½ volume, partition between ethyl acetate (500 mL) and saturated aqueous ammonium chloride (500 mL), separate layers, wash organic with saturated aqueous ammonium chloride (2×500 mL), and brine (300 mL). Dry with sodium sulfate, filter, and concentrate in vacuo to give 25.5 g of 2,3-dibromo-benzo[b]thiophen-6-ol (100%).

WORKUP

后处理

  1. temperatureheat
  2. temperatureto reflux for 4 hours
  3. concentrationConcentrate in vacuo
  4. custompartition between ethyl acetate (500 mL) and saturated aqueous ammonium chloride (500 mL)
  5. customseparate layers
  6. washwash organic with saturated aqueous ammonium chloride (2×500 mL), and brine (300 mL)
  7. dry with materialDry with sodium sulfate
  8. filtrationfilter
  9. concentrationconcentrate in vacuo