반응 #63988

반응 방정식

Rochelle's salt

sodium hydroxide

lithium aluminium hydride

oxime

1-acetyl-1-(3,4-dichlorophenyl)cyclobutane oxime

→

1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine

용매

water

ether

ether

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도under reflux for one hour
3. 3
   온도after cooling
4. 4
   추출continuously extracted with ether during eighteen hours
5. 5
   추출The ether extract
6. 6
   기타was dried
7. 7
   기타the ether removed

실험 절차

A solution of the oxime prepared above (4.0 g) in ether (50 ml) was added slowly to a stirred suspension of lithium aluminium hydride (0.9 g) in ether (50 ml) under nitrogen. The mixture was heated under reflux for one hour and, after cooling, water and then a 20% aqueous solution of Rochelle's salt (potassium sodium tartrate tetrahydrate) (27 ml) and a 10% aqueous solution of sodium hydroxide (6 ml) added. The reaction mixture was stirred for one hour and then continuously extracted with ether during eighteen hours. The ether extract was dried and the ether removed to leave a solid from which 1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine was separated by high pressure liquid chromatography. The product was identified by standard analytical techniques as the compound of Example 1 in the form of its free base.

출처