HRID264411
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 16 g of 6-hydroxy-1-indanone, 22.3 ml of 3-buten-2-ol and 160 mg of p-toluenesulfonic acid in 170 ml of 2,2-dimethoxy-propane was boiled under reflux for 38 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/ethyl acetate 4:1). In addition to 7.5 g of educt, there were obtained 6.21 g (28%) of (RS)-2-(2-buten-1-yl)-6-hydroxy-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/ethyl acetate 4:1)
- additionIn addition to 7.5 g of educt