HRID1900239

反应详情

EQUATION

反应方程式

HRID 1900239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anhydrous ferric chloride 10.42 g, 0.0026 mole) and benzoyl chloride II-1(29.65 g, were dissolved in CCl4 (40 ml and added dropwise with methyl furan-2-carboxylate I-1 (24 g. 0.19 mole). The reaction mixture was then heated under refluxing for 16 hrs, and after cooling was added with water(120 ml). The mixture was extracted with CCl4 , then the CCl4 layer was washed with water, 5% sodium bicarbonate solution, and then with water, till neutral, then dried over anhydrous Magnesium sulfate and filtered. The solvent of the filtrate was evaporated under reduced pressure, the residue was recrystallized from isopropanol, and then from methanol to give compound V-1. Yield 18.75 g(42.9%).

WORKUP

后处理

  1. temperatureThe reaction mixture was then heated
  2. temperatureunder refluxing for 16 hrs
  3. temperatureafter cooling
  4. extractionThe mixture was extracted with CCl4
  5. washthe CCl4 layer was washed with water, 5% sodium bicarbonate solution
  6. dry with materialwith water, till neutral, then dried over anhydrous Magnesium sulfate
  7. filtrationfiltered
  8. customThe solvent of the filtrate was evaporated under reduced pressure
  9. customthe residue was recrystallized from isopropanol
  10. customfrom methanol to give compound V-1