HRID1194951

反应详情

EQUATION

反应方程式

HRID 1194951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A 3 l glass reaction vessel was charged with 186 grams (1.0 mol) of 4,4'-dihydroxybiphenyl, 438 grams (2.6 mols) of m-dinitrobenzene, 363 grams of potassium carbonate and 2,000 ml of N,N-dimethylformamide. The mixture was reacted at a temperature of 140°-150° C. for 16 hours. After completing the reaction, the resultant mixture was cooled and filtered to remove potassium nitrite. The solvent was distilled off from the filtrate under reduced pressure. The residue was cooled to 65° C., added with 2,000 ml of methanol and stirred for an hour. The resulting crystals were filtered, washed with water, washed with methanol and dried to obtain 426 grams (99.5% yield) of 4,4'-bis(3-nitrophenoxy)biphenyl as brown crystals.

WORKUP

后处理

  1. customThe mixture was reacted at a temperature of 140°-150° C. for 16 hours
  2. customthe reaction
  3. filtrationfiltered
  4. customto remove potassium nitrite
  5. distillationThe solvent was distilled off from the filtrate under reduced pressure
  6. additionadded with 2,000 ml of methanol
  7. filtrationThe resulting crystals were filtered
  8. washwashed with water
  9. washwashed with methanol
  10. customdried