反应 #92977

反应方程式

hydrochloride hydrate

1-(2-chlorophenoxy)-2-hydroxybutyl chloride

1,2,3,4-tetrahydroisoquinoline

→

1-(2-Chlorophenoxy)-4-(1,2,3,4-tetrahydroisoquinolyl)-2-butanol Hydrochloride Hydrate

溶剂

n-butanol

反应条件

后处理

1. 1
   workup.ADDITIONA mixture of 11.8 g
2. 2
   过滤The reaction mixture was filtered at room temperature
3. 3
   workup.ADDITIONthe filtrate was mixed with 200 ml
4. 4
   萃取3N hydrochloric acid and extracted twice with 100 ml
5. 5
   萃取extracted with isopropyl ether
6. 6
   workup.ADDITIONtreated with ethereal hydrogen chloride
7. 7
   其他Recrystallization with isopropanol
8. 8
   其他yielded 6 g

实验过程

A mixture of 11.8 g. (0.05 mole) of 1-(2-chlorophenoxy)-2-hydroxybutyl chloride, 13.3 g. (0.1 mole) of 1,2,3,4-tetrahydroisoquinoline and 100 ml. of n-butanol was heated in a steel bomb at 120° C. for 24 hr. The reaction mixture was filtered at room temperature, the filtrate was mixed with 200 ml. 3N hydrochloric acid and extracted twice with 100 ml. isopropyl ether. The aqueous acidic solution was made basic and extracted with isopropyl ether and treated with ethereal hydrogen chloride. Recrystallization with isopropanol yielded 6 g. of the hydrochloride hydrate of the product which melted at 118°-120° C.

来源