HRID2296370

反应详情

EQUATION

反应方程式

HRID 2296370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
185 °C

PROCEDURE

实验过程

To a solution of 102 parts of anhydrous zinc chloride in 153 parts of 36% w/w aqueous hydrochloric acid and 200 parts of water are added 140 parts of aniline and 136 parts of 6-hydroxy-6-methyl-2-heptylamine hydrochloride (heptaminol hydrochloride). The whole is charged to a 1 liter tantalum-lined autoclave and stirred at 185° C. for 24 hours. The reaction mixture, after being discharged from the autoclave, is added to a hot solution of 750 parts sodium hydroxide in 1500 parts of water and stirred until cool. The organic phase is extracted with diethylether, washed with water, evaporated and distilled under reduced pressure. After recovering 58 parts of aniline there are obtained 135 parts of 2-amino-6-(4-amino-phenyl)-6-methyl-heptane boiling point 138°-40° C./65 Pa (82% yield based on heptaminol).

WORKUP

后处理

  1. stirringstirred
  2. temperatureuntil cool
  3. extractionThe organic phase is extracted with diethylether
  4. washwashed with water
  5. customevaporated
  6. distillationdistilled under reduced pressure
  7. customAfter recovering 58 parts of aniline