HRID1699675

反应详情

EQUATION

反应方程式

HRID 1699675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

3-amino-4-(benzylamino) quinoline (9.5 g; 0.038 mol) and glycolic acid (6.8 g; 0.089 mol) were mixed and the mixture was heated at 150° C. for about 4 hr. The dark mixture was then dissolved in dilute hydrochloric acid with heating. Upon cooling a precipitate formed and was filtered from the mixture. The solid was dissolved in hot water. The solution was then made basic with ammonium hydroxide to precipitate the product. A second, less pure, small crop was obtained from the original filtrate by making it basic with ammonium hydroxide. The solid was triturated in ethyl acetate to give a green colored powder. Total yield was 82%. The product was recrystallized from methanol to give a pure sample m.p. 211-213° C. Analysis: Calculated: C, 74.7; H, 5.2; N, 14.5. Found: C, 74.4; H, 5.1; N, 14.4.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureUpon cooling
  3. customa precipitate formed
  4. filtrationwas filtered from the mixture
  5. dissolutionThe solid was dissolved in hot water
  6. customto precipitate the product
  7. customA second, less pure, small crop was obtained from the original filtrate
  8. customThe solid was triturated in ethyl acetate
  9. customto give a green colored powder
  10. customThe product was recrystallized from methanol
  11. customto give a pure sample m.p. 211-213° C