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
4-methyl-3-{[5-(pyrrolidin-1-ylmethyl)pyridin-3-yl]ethyl}benzoic acid can be prepared in a manner similar to that described above for the Sonogashira reaction. 3-Ethynyl-5-<pyrrolidin-1-ylmethyl)pyridine and 3-iodo-4-methylbenzoic acid are used as coupling partners. Alternatively, the solvent (DMF) can be replaced by ethyl acetate and the base (Hunig base) can be replaced by triethylamine. The product can be isolated by filtration of the crude reaction mixture. The filter cake is washed sequentially with a solvent such as ethyl acetate and then water, then dried in a vacuum oven. Further purification can be achieved by slurrying the solids in water adjusted to pH 3 with the addition of concentrated HCl. After filtration and water wash, the product can be dried in a vacuum oven.
WORKUP
后处理
- customthat described above for the Sonogashira reaction
- customThe product can be isolated by filtration of the crude
- customreaction mixture
- washThe filter cake is washed sequentially with a solvent such as ethyl acetate
- dry with materialwater, then dried in a vacuum oven
- customFurther purification
- additionadjusted to pH 3 with the addition of concentrated HCl
- filtrationAfter filtration and water
- washwash
- customthe product can be dried in a vacuum oven