HRID472133

反应详情

EQUATION

反应方程式

HRID 472133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

76 g (216 mmol) of the sodium salt of 4-(2-methylquinolin-4-ylmethoxy)benzenesulfonic acid in 500 ml of dimethylformamide are added dropwise to a solution of 55 ml (649 mmol) of oxalyl chloride in 100 ml of dichloromethane, cooled beforehand to −10° C. After the addition, the reaction medium is stirred at ambient temperature for 18 h. The reaction medium is then poured into 11 of ice and then extracted with ethyl acetate. The organic phases are combined, washed with water and then with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, filtered and concentrated under vacuum. 77 g (92%) of 4-(2-methylquinolin-4-ylmethoxy)benzenesulfonyl chloride hydrochloride are obtained in the form of a beige solid.

WORKUP

后处理

  1. additionAfter the addition
  2. additionThe reaction medium is then poured into 11 of ice
  3. extractionextracted with ethyl acetate
  4. washwashed with water
  5. dry with materialwith a saturated aqueous solution of sodium chloride, dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum