HRID745142

反应详情

EQUATION

反应方程式

HRID 745142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Stannous chloride dihydrate (8 g) was added to a solution of 2,2'-bis(trifluoromethyl)-4,4'-dinitro-1,1'-biphenyl (1.9 g) in 5 ml of ethanol. Concentrated hydrochloric acid (12 ml) was added carefully to the mixture while stirring at room temperature. The mixture was refluxed overnight and the ethanol was removed. Water was added to the residue and it was made basic with 20% sodium hydroxide solution. The resulting white precipitate was collected by filtration, washed with water, dried and then extracted in a Soxhlet flask with acetone for four hours. Removal of acetone gave a white residue, 2,2'-bis(trifluoromethyl)-4,4'-diamino-1,1'-biphenyl, ##STR7## which was recrystallized from chloroform-hexane to give 1.2 g (74% yield) of short white needles, m.p. 185°-186° C.

WORKUP

后处理

  1. temperatureThe mixture was refluxed overnight
  2. customthe ethanol was removed
  3. additionWater was added to the residue and it
  4. filtrationThe resulting white precipitate was collected by filtration
  5. washwashed with water
  6. customdried
  7. extractionextracted in a Soxhlet flask with acetone for four hours
  8. customRemoval of acetone