HRID963068
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed overnight
- customThe solvent was evaporated
- additionethyl acetate and a saturated aqueous sodium hydrogencarbonate solution were added
- washwashed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- filtrationThe resulting crystals were collected by filtration
- washwashed with ethyl acetate