HRID64890
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 18.2 g of 1-(2-aminobenzoyl)piperidine and 12.2 g of 2-methyl-4-chloropyridine in 5.0 ml of acetic acid was heated at reflux for six hours and then kept at room temperature overnight. The reaction mixture was concentrated in vacuo, and the residue treated with dilute acid to pH 2 and extracted with methylene dichloride. The aqueous layer was made basic with potassium carbonate and extracted with chloroform. Further work-up of this solution afforded 2.58 g of 1-[2-(2-methyl-4-pyridinylamino)benzoyl]piperidine, m.p. 93°-95° C. when recrystallized from ethyl acetate--ether--hexane.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for six hours
- concentrationThe reaction mixture was concentrated in vacuo
- additionthe residue treated
- additionwith dilute acid to pH 2
- extractionextracted with methylene dichloride
- extractionextracted with chloroform