HRID2119695
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
Under a nitrogen stream, a solution of 0.48 g of 2,5-di-t-butyl-4-trimethylacetoxy-1-(2-methyl-2-propenyloxy)benzene in 5 ml of dimethylaniline was refluxed overnight. The solution was allowed to attain room temperature and concentrated under reduced pressure, then extracted with ethyl acetate and 5% hydrochloric acid. The organic layers were washed with saturated brine, dried over anhydrous magnesium sulfate, and then concentrated. The concentrate was purified by silica gel column chromatography (in n-hexane containing 0.5% ethyl acetate) to give 0.43 g of 4,7-di-t-butyl-2,2-dimethyl-5-trimethylacetoxy-2,3-dihydrobenzofuran as a colorless solid.
WORKUP
后处理
- customto attain room temperature
- concentrationconcentrated under reduced pressure
- extractionextracted with ethyl acetate and 5% hydrochloric acid
- washThe organic layers were washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe concentrate was purified by silica gel column chromatography (in n-hexane containing 0.5% ethyl acetate)