HRID264384
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
A solution of 9.1 g of 6-ethyl-3,3-dimethyl-1-indanone, 9.98 ml of 3-buten-2-ol and 250 mg of p-toluenesulfonic acid in 100 ml of 2,2-dimethoxypropane was boiled under reflux for 88 hours on a water separator filled with molecular sieve (0.4 nm, 2 mm pearl shaped). The reaction mixture was subsequently concentrated in a vacuum and purified by column chromatography on silica gel (hexane/diethyl ether 6:1). In addition to 2.0 g of educt, there were obtained 8.2 g (70%) of (RS)-2-(2-buten-1-yl)-6-ethyl-3,3-dimethyl-1-indanone as a yellow oil.
WORKUP
后处理
- additionseparator filled with molecular sieve (0.4 nm, 2 mm pearl shaped)
- concentrationThe reaction mixture was subsequently concentrated in a vacuum
- custompurified by column chromatography on silica gel (hexane/diethyl ether 6:1)
- additionIn addition to 2.0 g of educt