HRID2166623
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 2.0 g. (4.57 mmols.) of 3-[4-(1,1-dimethylheptyl)-2-hydroxyphenyl]-4-(3-phenylpropyl)-4-piperidinol, 0.95 g. (5.0 mmols.) of p-toluenesulfonic acid monohydrate and 100 ml. of toluene is heated under reflux for 2 hours with a Dean Stark trap. The reaction mixture is cooled and added to 100 ml. of 20% potassium carbonate-200 ml. dichloromethane. The dichloromethane extract along with two additional 200 ml. dichloromethane extracts of the basic phase is dried over magnesium sulfate and evaporated. The residue is crystallized from ether-pentane to yield the title compound.
WORKUP
后处理
- additionA mixture of 2.0 g
- temperatureunder reflux for 2 hours with a Dean Stark trap
- temperatureThe reaction mixture is cooled
- additionadded to 100 ml
- extractionThe dichloromethane extract along with two additional 200 ml
- dry with materialdichloromethane extracts of the basic phase is dried over magnesium sulfate
- customevaporated
- customThe residue is crystallized from ether-pentane