HRID1287547

反应详情

EQUATION

反应方程式

HRID 1287547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

158 parts of pyridine and 155 parts of benzoyl chloride are heated with 4 parts of copper powder for an hour at 100° to 105° C. At 70° to 80° C there is then added 197 parts of methylbenzylaniline and heating is continued for another five hours at 100° to 105° C. When the reaction is over 800 parts of toluene is added at 70° to 80° C, and the precipitate is suction filtered and dissolved in 1,000 parts of 5% hydrochloric acid. The product is clarified with animal charcoal and reprecipitated in the cold with ammonia and recrystalized from a mixture of ethanol and water for further purification. 50 parts of 4-(4'-methylbenzylaminophenyl)-pyridine is obtained as practically colorless crystals which melt at 118° to 119° C.

WORKUP

后处理

  1. temperatureheating
  2. additionis added at 70° to 80° C
  3. filtrationfiltered
  4. dissolutiondissolved in 1,000 parts of 5% hydrochloric acid
  5. customreprecipitated in the cold with ammonia
  6. customrecrystalized from a mixture of ethanol and water for further purification