HRID644405

反应详情

EQUATION

反应方程式

HRID 644405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-acetylsalicylic acid methyl ester (13.59 g, 70 mmol), benzyl bromide (17.96 g, 105 mmol), potassium carbonate (19.35 g, 140 mmol) and methyl ethyl ketone (350 mL) was refluxed for 8 hours. After cooling, the solvent was evaporated under reduced pressure. 2N Hydrochloric acid was added to the residue, and it was extracted with ethyl acetate. After the ethyl acetate layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated, the residue was recrystallized from isopropyl ether to give the title compound (14.20 g, 71.4%) as a white solid.

WORKUP

后处理

  1. temperaturewas refluxed for 8 hours
  2. temperatureAfter cooling
  3. customthe solvent was evaporated under reduced pressure
  4. addition2N Hydrochloric acid was added to the residue, and it
  5. extractionwas extracted with ethyl acetate
  6. washAfter the ethyl acetate layer was washed with water and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated
  9. customthe residue was recrystallized from isopropyl ether