HRID930960
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 mixture comprising 217 g (1.00 mol) 8-methoxy-8-(methoxymethyl)-1,4-dioxaspiro[4.5]decane (prepared according to intermediate example 16e), 1.7 L acetone, 0.86 L water and 30.5 g 4-methylbenzenesulfonic acid hydrate was stirred at 23° C. overnight. The acetone was removed, 0.5 L saturated aqueous sodium hydrogencarbonate added followed by 0.4 L brine. The mixture was extracted with ethyl acetate, the combined organic layers were washed with brine and dried over sodium sulfate. After filtration and removal of the solvent 180 g (max. 100%) of the title compound were obtained that was used without further purification.
WORKUP
后处理
- customThe acetone was removed
- addition0.5 L saturated aqueous sodium hydrogencarbonate added
- extractionThe mixture was extracted with ethyl acetate
- washthe combined organic layers were washed with brine
- dry with materialdried over sodium sulfate
- filtrationAfter filtration and removal of the solvent 180 g (max. 100%) of the title compound
- customwere obtained
- customthat was used without further purification