HRID981000

反应详情

EQUATION

反应方程式

HRID 981000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension containing 16 g of the sulfonamide of Example 3, 7.7 g of potassium carbonate and 6.7 g of n-butylisocyanate in 130 of 2-butanone was refluxed for 4 hours, then stirred overnight at room temperature. After concentrating the mixture in vacuo, the residue was diluted with about 150 ml of water and the solution was washed 1×100 ml of ethyl ether. The aqueous layer was acidified with concentrated hydrochloric acid (red to litmus paper) and the resulting suspension was filtered, the suction-dried overnight to give 20 g of the subject compound; m.p. 156°-159° C. IR (nujol): 1680 cm-1 (C=O).

WORKUP

后处理

  1. temperaturewas refluxed for 4 hours
  2. concentrationAfter concentrating the mixture in vacuo
  3. additionthe residue was diluted with about 150 ml of water
  4. washthe solution was washed 1×100 ml of ethyl ether
  5. filtrationthe resulting suspension was filtered