HRID2372413
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
2-Benzyloxymethyl-2-cyclohexyl-propan-1,3-diol(3 g.),2,2-dimethoxypropane (8 ml), p-toluenesulphonic acid (150 mg.) and molecular sieves (type 4A) were heated in refluxing dry toluene (50 ml.) for four hours. The mixture was cooled and filtered. The filtrate was diluted with ether and the ethereal solution was extracted with aqueous sodium hydrogen carbonate solution. The ethereal solution was washed with water, dried over anhydrous magnesium sulphate and evaporated in vacuo. The residue was purified by chromatography on silica, eluting with 1:5 ether:hexane. 5-Benzyloxymethyl-5-cyclohexyl-2,2-dimethyl-1,3-dioxane(3.0 g) was obtained as a colourless oil.
WORKUP
后处理
- temperatureThe mixture was cooled
- filtrationfiltered
- additionThe filtrate was diluted with ether
- extractionthe ethereal solution was extracted with aqueous sodium hydrogen carbonate solution
- washThe ethereal solution was washed with water
- dry with materialdried over anhydrous magnesium sulphate
- customevaporated in vacuo
- customThe residue was purified by chromatography on silica
- washeluting with 1:5 ether