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
PROCEDURE
实验过程
Cesium carbonate (176 g, 1.13 mol) was added to a solution of 5-acetoxy-2-(5-methyltetrazol-1-yl)benzoic acid (164 g, 0.620 mol) in 1.8 L of acetone. The mixture was stirred vigorously and iodoethane (116 g, 0.682 mol) diluted with 100 mL of acetone was added dropwise over a one-hour period. The reaction was stirred overnight at ambient temperature and was then concentrated under reduced pressure. The resulting solid was partitioned between dichloromethane and water. The aqueous fraction was extracted with dichloromethane and the combined organic fractions were dried over sodium sulfate, filtered, and concentrated to give 166 g of ethyl 5-acetoxy-2-(5-methyltetrazol-1-yl)benzoate as a brown oil.
WORKUP
后处理
- additionwas added dropwise over a one-hour period
- stirringThe reaction was stirred overnight at ambient temperature
- concentrationwas then concentrated under reduced pressure
- customThe resulting solid was partitioned between dichloromethane and water
- extractionThe aqueous fraction was extracted with dichloromethane
- dry with materialthe combined organic fractions were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated