反应详情

To a solution of 8 g (0.51 mole) of methyl 4-oxocyclohexane-1-carboxylate in 50 ml of dry benzene is added 4 g (0.064 mole) of ethylene glycol and 0.10 g of p-toluenesulfonic acid and this mixture is refluxed overnight with a Dean-Stark apparatus. The cooled reaction is allowed to stand and the bottom layer (ethylene glycol) separated and the remaining benzene layer washed with aqueous sodium bicarbonate, dried over MgSO4, and stripped to dryness, giving methyl 1,4-dioxaspiro[4,5]decane-8-carboxylate as a clear liquid residue. This material is used without further purification in the next step.

1. temperaturethis mixture is refluxed overnight with a Dean-Stark apparatus
2. customThe cooled reaction
3. customthe bottom layer (ethylene glycol) separated
4. washthe remaining benzene layer washed with aqueous sodium bicarbonate
5. dry with materialdried over MgSO4