HRID1577932

反应详情

EQUATION

反应方程式

HRID 1577932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 78 g of 8-(2-propynyloxy)-5-hydroxy-3,4-dihydrocarbostyril were added 102 g of epichlorohydrin, 60 g of potassium carbonate and 600 ml of methanol, and the resulting mixture was heated while refluxing for 2.5 hours on a water bath. After completion of the reaction, the methanol was evaporated, and water was added to the residue followed by extracting with chloroform. The chloroform layer was washed with water and dried over anhydrous sodium sulfate. The chloroform was evaporated under reduced pressure, and the residual crystals were recrystallized from isopropanol to obtain 67 g of 8-(2-propynyloxy)-5-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril having a melting point of 142°-143.5° C.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperaturewhile refluxing for 2.5 hours on a water bath
  3. customAfter completion of the reaction
  4. customthe methanol was evaporated
  5. additionwater was added to the residue
  6. extractionby extracting with chloroform
  7. washThe chloroform layer was washed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe chloroform was evaporated under reduced pressure
  10. customthe residual crystals were recrystallized from isopropanol