HRID2057450

反应详情

EQUATION

反应方程式

HRID 2057450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2 liters of acetone and 500 ml of water were added to 150 g of 5,8-dihydroxy-3,4-dihydrocarbostyril, and 138 g of potassium carbonate and 150 g of 2-propynyl bromide were further added thereto. The resulting mixture was heated while refluxing for 3 hours on a water bath. After completion of the reaction, the acetone and the 2-propynyl bromide were evaporated under reduced pressure, and the residue was made acidic with concentrated hydrochloric acid. The mixture was extracted with chloroform, and 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-diethyl ether to obtain 110 g of 8-(2-propynyloxy)-5-hydroxy-3,4-dihydrocarbostyril having a melting point of 141°-142° C.

WORKUP

后处理

  1. additionwere further added
  2. temperatureThe resulting mixture was heated
  3. temperaturewhile refluxing for 3 hours on a water bath
  4. customAfter completion of the reaction
  5. customthe acetone and the 2-propynyl bromide were evaporated under reduced pressure
  6. extractionThe mixture was extracted 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-diethyl ether