HRID2417513

反应详情

EQUATION

反应方程式

HRID 2417513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

5.0 g (29 mmol) of 4-methoxy-1-methyl-2-nitrobenzene was added to a mixture of 50 ml of benzene, 50 ml of perbenzoic acid and 8 g (45 mmol) of N-bromosuccinimide, and they were stirred at 80° C. for one day. After the treatment with ethyl acetate as the extracting solvent by an ordinary method, the obtained crude product was dissolved in 50 ml of ethanol. 8.4 g (60 mmol) of glycine ethyl ester hydrochloride and 5.0 g (60 mmol) of sodium hydrogencarbonate were added to the obtained solution, and they were stirred at 70° C. overnight. The solvent was evaporated. After the extraction with ethyl acetate, the extract was washed with 1 N hydrochloric acid. The obtained aqueous layer was made basic with 1 N sodium hydroxide. After the extraction with ethyl acetate, the obtained organic layer was washed with saturated aqueous sodium chloride solution and then dried. The solvent was evaporated to obtain the title compound.

WORKUP

后处理

  1. stirringwere stirred at 70° C. overnight
  2. customThe solvent was evaporated
  3. extractionAfter the extraction with ethyl acetate
  4. washthe extract was washed with 1 N hydrochloric acid
  5. extractionAfter the extraction with ethyl acetate
  6. washthe obtained organic layer was washed with saturated aqueous sodium chloride solution
  7. customdried
  8. customThe solvent was evaporated