HRID659934

反应详情

EQUATION

反应方程式

HRID 659934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1H-tetrazol (0.45 g) and ethyl 3-(2-bromoethoxy)-2,4-dichlorobenzoate (2.00 g) were suspended in DMF (15 ml), potassium carbonate (1.21 g) and sodium iodide (0.04 g) were added thereto and the mixture was stirred at 80° C. for 3 hours. After the reaction, cool water was added, extracted with ethyl acetate (100 ml) and dried over anhydrous magnesium sulfate. The residue obtained by distilling off ethyl acetate was purified with silica gel column chromatography (elution solvent; ethyl acetate: hexane=1:1) to obtain the desired ethyl 2,4-dichloro-3-[2-(1H-tetrazol-1-yl)ethoxy]benzoate (0.88 g) and ethyl 2,4-dichloro-3-[2-(1H-tetrazol-2-yl)ethoxy]benzoate (0.99 g).

WORKUP

后处理

  1. customAfter the reaction
  2. additionwas added
  3. extractionextracted with ethyl acetate (100 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe residue obtained
  6. distillationby distilling off ethyl acetate
  7. customwas purified with silica gel column chromatography (elution solvent; ethyl acetate: hexane=1:1)