HRID1654487
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 of dimeric 2-hydroxycyclohexanone (13.7 g), 2 benzyloxyethanol (20 g) and p-toluensulphonic acid (2 g) were dissolved in xylene (500 ml) in a round bottom flask fitted with a Dean Stark apparatus and reluxed for 10 hrs. The resulting solution was cooled, washed with sodium hydrogen carbonate (3×50 ml) dried and concentrated under reduced pressure. The crude oil was then purified by flash chromatography using cyclohexane/ethyl acetate 60/40 as eluant yielding 20 g of the title compound (Rf=0.5).
WORKUP
后处理
- customfitted with a Dean Stark apparatus
- temperatureThe resulting solution was cooled
- washwashed with sodium hydrogen carbonate (3×50 ml)
- customdried
- concentrationconcentrated under reduced pressure
- customThe crude oil was then purified by flash chromatography