HRID330449

反应详情

EQUATION

反应方程式

HRID 330449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.5 g of ethyl chloroformate in 10 ml of anhydrous acetonitrile is dropwise added to a solution of 5.5 g of 2-aminobenzenesulfonamide and 2.5 g of pyridine in 80 ml of anhydrous acetonitrile at room temperature during 2 hours. After stirring at room temperature, the mixture is poured into ice water and acidified with 100 ml of 2N-hydrochloric acid solution. The mixture is extracted with ethyl acetate twice, washed with an aqueous saturated sodium hydrogen carbonate and then with a saturated brine, and dried over anhydrous sodium sulfate. Then the mixture is concentrated under reduced pressure. The residue is crystallized from chloroform to give 6.6 g of the title compound.

WORKUP

后处理

  1. extractionThe mixture is extracted with ethyl acetate twice
  2. washwashed with an aqueous saturated sodium hydrogen carbonate
  3. dry with materialwith a saturated brine, and dried over anhydrous sodium sulfate
  4. concentrationThen the mixture is concentrated under reduced pressure
  5. customThe residue is crystallized from chloroform