HRID1108634

反应详情

EQUATION

反应方程式

HRID 1108634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

30 mg (0.0695 mmol) of 4-benzylamino-1-[3-(tert-butoxycarbonylamino)propyl]-1H-imidazo[4,5-c]quinoline was dissolved in 3 ml of formic acid. 0.1 g of 20% palladium hydroxide-carbon was added thereto and the mixture was refluxed under heating for one day. The reaction mixture was filtered and the filtrate was evaporated to distill off the solvent under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform: methanol:32% acetic acid=6:3:1 (v/v)) to obtain the acetic acid salt of the object. The thus obtained product was subjected to treatment with alkali to obtain the free base. The precipitate thus formed was collected by filtration to obtain 7 mg (0.0290 mmol) of 1-(3-aminopropyl)-1H-imidazo[4,5-c]quinoline-4-amine shown below as faint brown powder. ##STR40## The physicochemical data of this compound was in agreement with compound of Example 5.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for one day
  3. filtrationThe reaction mixture was filtered
  4. customthe filtrate was evaporated
  5. distillationto distill off the solvent under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography (chloroform: methanol:32% acetic acid=6:3:1 (v/v))
  7. customto obtain the acetic acid salt of the object
  8. customto obtain the free base
  9. customThe precipitate thus formed
  10. filtrationwas collected by filtration