HRID280853

反应详情

EQUATION

反应方程式

HRID 280853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-(3-aminopropyl)-4-benzhydrylpiperazine (1.55 g) and triethylamine (0.7 ml) in chloroform (15 ml) was dropwise added p-methoxybenzoyl chloride (0.85 g) at ambient temperature with stirring, which was continued for 20 minutes. The reaction mixture was washed successively with aqueous sodium bicarbonate and water. The organic layer was separated, dried and evaporated in vacuo. The resultant oily product was subjected to column chromatography on silica gel eluting with ethyl acetate. The fractions containing the desired compound were combined and evaporated in vacuo. The residue was crystallized from a mixture of ethyl acetate and hexane to give 1-[3-(4-methoxybenzoylamino)propyl]-4-benzhydrylpiperazine (1.1 g) as white crystals. mp: 126°-128° C.

WORKUP

后处理

  1. customat ambient temperature
  2. washThe reaction mixture was washed successively with aqueous sodium bicarbonate and water
  3. customThe organic layer was separated
  4. customdried
  5. customevaporated in vacuo
  6. additionThe fractions containing the desired compound
  7. customevaporated in vacuo
  8. customThe residue was crystallized from a mixture of ethyl acetate and hexane