HRID1721879
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
Ethyl 4-[2-(2-n-propylimidazol-1-yl)propoxy]-3-ketobutanoate (590 mg), 3-aminocyclohex-2-enone (220 mg) and 2-chlorobenzaldehyde (281 mg) were stirred in refluxing ethanol (8 ml) for 8 hours. The solvent was removed under reduced pressure. The crude product was chromatographed over silica eluting with a mixture of diethylamine and ethyl acetate (1:49). The solvents were removed in vacuo and the residue rechromatographed over silica eluting with a mixture of methanol and ethyl acetate [1:9]. The solvents were removed in vacuo. The resulting foam was stirred in ether overnight, the solid filtered and dried in vacuo yielding the title compound as a white solid 220 mg (22%). M.p. 127°-131° C.
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- customThe crude product was chromatographed over silica eluting with a mixture of diethylamine and ethyl acetate (1:49)
- customThe solvents were removed in vacuo
- customthe residue rechromatographed over silica eluting with a mixture of methanol and ethyl acetate [1:9]
- customThe solvents were removed in vacuo
- filtrationthe solid filtered
- customdried in vacuo