HRID1269850

反应详情

EQUATION

反应方程式

HRID 1269850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

Potassium carbonate (1.16 g, 8.39 mmol) was added to a solution of 5-fluoro-2-nitrotoluene (1.0 g, 6.45 mmol) and methyl salicylate (1.18 g, 7.74 mmol) in N,N-dimethylformamide (8 ml), and the resulting mixture was stirred at 140° C. for 1 hour. After the reaction, the reaction solution was cooled to 0° C. and a saturated aqueous sodium chloride solution was added thereto, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. The organic layer dried was concentrated and then purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=10/1) to obtain methyl 2-(3-methyl-4-nitrophenoxy)benzoate (1.88 g, 85%).

WORKUP

后处理

  1. customAfter the reaction
  2. temperaturethe reaction solution was cooled to 0° C.
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materiala saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate
  6. customThe organic layer dried
  7. concentrationwas concentrated
  8. custompurified by a silica gel column chromatography (eluent: hexane/ethyl acetate=10/1)