HRID49946

反应详情

EQUATION

反应方程式

HRID 49946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.00 g (36.2 mmol) of potassium carbonate and 3.27 g (26.6 mmol) of isopropyl bromide were added to a mixture of 2.00 g (13.2 mmol) of methyl salicylate and 10 ml of dimethylformamide, and they were stirred at room temperature overnight and then at 70° C. for 4 hours. 12.0 ml (36 mmol) of 3 M aqueous sodium hydroxide solution and 6.0 ml of ethanol were added to the reaction mixture, and they were stirred at 80° C. for 6 hours and then concentrated under reduced pressure. Water was added thereto. After washing with ethyl acetate, the aqueous layer was neutralized with hydrochloric acid. After the extraction with ethyl acetate, the extract was washed with water and saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain the title compound.

WORKUP

后处理

  1. waitat 70° C. for 4 hours
  2. stirringwere stirred at 80° C. for 6 hours
  3. concentrationconcentrated under reduced pressure
  4. additionWater was added
  5. washAfter washing with ethyl acetate
  6. extractionAfter the extraction with ethyl acetate
  7. washthe extract was washed with water and saturated aqueous sodium chloride solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure