HRID659934
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter the reaction
- additionwas added
- extractionextracted with ethyl acetate (100 ml)
- dry with materialdried over anhydrous magnesium sulfate
- customThe residue obtained
- distillationby distilling off ethyl acetate
- customwas purified with silica gel column chromatography (elution solvent; ethyl acetate: hexane=1:1)