HRID343794

反应详情

EQUATION

反应方程式

HRID 343794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tin (II) chloride dihydrate (346.3 g, 1.54 mol) was added to a solution of 2,3,6,7-tetrachloro-5-nitro-quinoxaline (96.2 g, 0.31 mol) in ethyl acetate (1.8 l). The mixture was heated under reflux for 4 hours, cooled and poured cautiously into an excess of aqueous saturated sodium bicarbonate. The mixture was filtered through "Celite", (Trade Mark), washing well with ethyl acetate. The filter cake was macerated with more ethyl acetate and the solid material filtered off. The combined ethyl acetate solutions were dried (MgSO4) and concentrated under reduced pressure to give 5-amino-2,3,6,7-tetrachloroquinoxaline (73.4 g, 84%) as a yellow solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. temperaturecooled
  4. filtrationThe mixture was filtered through "Celite", (Trade Mark),
  5. washwashing well with ethyl acetate
  6. filtrationthe solid material filtered off
  7. dry with materialThe combined ethyl acetate solutions were dried (MgSO4)
  8. concentrationconcentrated under reduced pressure