HRID1060686

反应详情

EQUATION

反应方程式

HRID 1060686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of N-[4-(4-amino-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-1-yl)butyl]acetamide (˜2.1 g) in 6 N hydrochloric acid (30 mL) was sealed in a flask and then heated at 100° C. for about 30 hours. The reaction mixture was allowed to cool to ambient temperature and then filtered to remove any particulates. The filtrate was made basic (pH 14) with 25% sodium hydroxide and then extracted with chloroform (×2). The aqueous layer was combined with sodium chloride (20 g) and then extracted with chloroform (×3). The organics were combined, washed with brine, dried over sodium sulfate and then concentrated under reduced pressure to provide 1.44 g of 1-(4-aminobutyl)-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine.

WORKUP

后处理

  1. temperatureto cool to ambient temperature
  2. filtrationfiltered
  3. customto remove any particulates
  4. extractionextracted with chloroform (×2)
  5. extractionextracted with chloroform (×3)
  6. washwashed with brine
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated under reduced pressure