HRID1638908

反应详情

EQUATION

反应方程式

HRID 1638908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 70 ml acetone mixture of 8.5 g of 4-ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide and 6.0 g of anhydrous potassium carbonate, added was 3.3 g of n-butylisocyanate at room temperature, followed by heating under reflux for 3 hours. After the reaction was completed, acetone was evaporated under reduced pressure, and then the residue was emptied into ice water to filter insolbles off, and then the filtrate was precipitated with hydrochloric acid. Crystals precipitated was filtered, washed with water and dried to obtain 10.8 g of N-(n-butylcarbamoyl)-4-ethoxycarbonyl-1-(2-pyridyl)pyrazole-5-sulfonamide. m.p.: 180° to 181° C.

WORKUP

后处理

  1. additionadded
  2. customat room temperature
  3. temperatureby heating
  4. temperatureunder reflux for 3 hours
  5. customacetone was evaporated under reduced pressure
  6. filtrationto filter insolbles off, and then the filtrate
  7. customwas precipitated with hydrochloric acid
  8. customCrystals precipitated
  9. filtrationwas filtered
  10. washwashed with water
  11. customdried