HRID1253262

反应详情

EQUATION

反应方程式

HRID 1253262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,3-Cyclopentane dicarboxylic acid (1.6 g., 10 mmole) and 1-(4-aminobutyl)-4-(2-quinolyl)piperazine (2.8 g., 10 mmole) were combined in 200 ml. of xylene and refluxed for 24 hours with water removal via a Dean-Stark trap. The solvent was then removed in vacuum and the residue redissolved in chloroform and filtered through 75 g. of silica gel. The column was rinsed with 5% ethanol/chloroform and the product-containing fractions were combined and evaporated. The residue was recrystallized from isopropanol with the addition of 4N isopropanolic HCl to give 820 mg. of the title compound as the dihydrochloride hemihydrate; m.p. 240°-242° C.

WORKUP

后处理

  1. customThe solvent was then removed in vacuum
  2. dissolutionthe residue redissolved in chloroform
  3. filtrationfiltered through 75 g
  4. washThe column was rinsed with 5% ethanol/chloroform
  5. customevaporated
  6. customThe residue was recrystallized from isopropanol with the addition of 4N isopropanolic HCl
  7. customto give 820 mg