HRID1493545
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customIn an eggplant flask having
- customa ground-in stopper and equipped with a condenser
- customas obtained in Preparation Example 3
- extractionThe mixture was extracted with benzene by means of a Soxhlet extractor
- customThe solvent was removed from the
- extractionextract by distillation under reduced pressure
- customthe resulting crude crystal was recrystallized from 99% ethanol