HRID1493545

反应详情

EQUATION

反应方程式

HRID 1493545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In an eggplant flask having a ground-in stopper and equipped with a condenser were charged 2-iodo-3-nitrotoluene (6) as obtained in Preparation Example 3 and an equivalent weight of a copper powder, and the contents were stirred in an oil bath at 200° C. for 10 hours. The mixture was extracted with benzene by means of a Soxhlet extractor. The solvent was removed from the extract by distillation under reduced pressure, and the resulting crude crystal was recrystallized from 99% ethanol to obtain 6,6'-dimethyl-2,2'-dinitro-1,1'-biphenyl (7) as a black needle-like crystal having a melting point of 107.4° to 108.3° C. and a 73% yield.

WORKUP

后处理

  1. customIn an eggplant flask having
  2. customa ground-in stopper and equipped with a condenser
  3. customas obtained in Preparation Example 3
  4. extractionThe mixture was extracted with benzene by means of a Soxhlet extractor
  5. customThe solvent was removed from the
  6. extractionextract by distillation under reduced pressure
  7. customthe resulting crude crystal was recrystallized from 99% ethanol