HRID1818131

反应详情

EQUATION

反应方程式

HRID 1818131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium hydroxide (25 g, 0.625 mol) in water (205 mL) was added to a solution of N-[7-bromo-4-(2-hydroxy-2-methylpropylamino)quinolin-3-yl]-2-ethoxyacetamide (170.88 g, 0.431 mol) in ethanol (700 mL), and the reaction was heated at reflux under a nitrogen atmosphere for two hours. Upon cooling the reaction, a precipitate formed and was isolated by filtration. The solid was purified by flash column chromatography on silica gel (eluting sequentially with chloroform, 99:1 chloroform:methanol, and 97:3 chloroform:methanol) to provide 80.31 g of 1-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)-2-methylpropan-2-ol as a tan solid.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureat reflux under a nitrogen atmosphere for two hours
  3. temperatureUpon cooling
  4. customthe reaction
  5. customa precipitate formed
  6. customwas isolated by filtration
  7. customThe solid was purified by flash column chromatography on silica gel (
  8. washeluting sequentially with chloroform, 99:1 chloroform