HRID2163594

反应详情

EQUATION

反应方程式

HRID 2163594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Concentrated sulfuric acid (1.5 ml.) is added to a slurry of 6,7-dimethoxy-2-aminoquinoline-3-carboxamide (5.0 g., 0.02 mole) and acetic anhydride (40 ml). The slurry dissolves to give a dark orange solution from which a heavy yellow precipitate separates. Acetic anhydride (10 ml.) is added to facilitate stirring and heating continued for an additional 75 minutes. The mixture is cooled, water (50 ml.) added and the resulting solution made alkaline with 5N sodium hydroxide (225 ml.). It is chilled, the precipitate collected by filtration and air-dried. The yellow solid is recrystallized from ethanol. Yield = 2.37 g., M.P. 300° -302° (dec.).

WORKUP

后处理

  1. dissolutionThe slurry dissolves
  2. customto give a dark orange solution from which a heavy yellow precipitate separates
  3. temperatureheating
  4. temperatureThe mixture is cooled
  5. temperatureIt is chilled
  6. filtrationthe precipitate collected by filtration
  7. customair-dried
  8. customThe yellow solid is recrystallized from ethanol