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
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
- stirringstirred
- temperatureuntil cool
- extractionThe organic phase is extracted with diethylether
- washwashed with water
- customevaporated
- distillationdistilled under reduced pressure
- customAfter recovering 58 parts of aniline