HRID963068

反应详情

EQUATION

反应方程式

HRID 963068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Amino-4-(2-chlorobenzoyl)thiophene-2-carboxylic acid (240 g), potassium carbonate (176 g) and ethyl iodide (150 ml) were added to acetone (5 l), and the mixture was refluxed overnight. The solvent was evaporated, and ethyl acetate and a saturated aqueous sodium hydrogencarbonate solution were added. The precipitated layer was taken out, washed with brine, dried over sodium sulfate and concentrated. The resulting crystals were collected by filtration and washed with ethyl acetate to give 126 g of ethyl 5-amino-4-(2-chlorobenzoyl)thiophene-2-carboxylate.

WORKUP

后处理

  1. temperaturethe mixture was refluxed overnight
  2. customThe solvent was evaporated
  3. additionethyl acetate and a saturated aqueous sodium hydrogencarbonate solution were added
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with ethyl acetate