HRID1089122

反应详情

EQUATION

反应方程式

HRID 1089122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N,N'-Carbonyldiimidazole (1.2 g) is added to a solution of 4,5-dihydroxyquinoline-3-carboxylic acid (0.7 g), which is prepared according to the method described in Japanese Patent First Publication No. 65874/1981, in dry dimethyl sulfoxide (30 ml) and the mixture is stirred at room temperature for 30 minutes. 4-(4-Diphenylmethyl-1-piperazinyl)butylamine (2.2 g) is added to the reaction mixture and the mixture is stirred at room temperature for 6 hours, and thereto is added water (about 200 ml), and the mixture is extracted with chloroform. The organic layer is dried over anhydrous magnesium sulfate and the solvent is distilled off. The residue is subjected to silica gel column chromatography, followed by elution with chloroform - methanol (30 : 1). The obtained crystals are recrystallized from isopropyl alcohol to give the desired compound (0.72 g). m.p. 215° to 218° C.

WORKUP

后处理

  1. customis prepared
  2. extractionthe mixture is extracted with chloroform
  3. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
  4. distillationthe solvent is distilled off
  5. washfollowed by elution with chloroform - methanol (30 : 1)
  6. customThe obtained crystals are recrystallized from isopropyl alcohol