HRID1721879

反应详情

EQUATION

反应方程式

HRID 1721879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed under reduced pressure
  2. customThe crude product was chromatographed over silica eluting with a mixture of diethylamine and ethyl acetate (1:49)
  3. customThe solvents were removed in vacuo
  4. customthe residue rechromatographed over silica eluting with a mixture of methanol and ethyl acetate [1:9]
  5. customThe solvents were removed in vacuo
  6. filtrationthe solid filtered
  7. customdried in vacuo