Reaktion #54280

Reaktionsgleichung

1-(3,4-methylenedioxyphenyl)-2-chloroethanol

ethylamine

→

1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   workup.DISTILLATIONthe ethanol and excess ethylamine are distilled off under reduced pressure
3. 3
   ExtraktionThe residue is extracted with 100 ml
4. 4
   Waschenof 1N HCl and the extract is washed twice with 100 ml
5. 5
   ExtraktionThe hydrochloric acid extract solution
6. 6
   Extraktionthe liberated oil is extracted with ether
7. 7
   ExtraktionThe ether extract
8. 8
   Sonstigeis dried
9. 9
   workup.ADDITIONan etherial hydrochloric acid solution is added
10. 10
    Filtrationare filtered off
11. 11
    Waschenwashed with ether
12. 12
    SonstigeUpon recrystallization from isopropyl alcohol 7.8 g

Vorschrift

19.5 g. of 1-(3,4-methylenedioxyphenyl)-2-chloroethanol are added to a solution of 170 g. of ethylamine in 200 ml. of cooled ethanol and the mixture is heated at 80° C. for 8 hours in an autoclave. After cooling, the ethanol and excess ethylamine are distilled off under reduced pressure. The residue is extracted with 100 ml. of 1N HCl and the extract is washed twice with 100 ml. of ether. The hydrochloric acid extract solution is made basic with 1N caustic soda and the liberated oil is extracted with ether. The ether extract is dried and an etherial hydrochloric acid solution is added thereto. The crystals which settle out on standing are filtered off and washed with ether. Upon recrystallization from isopropyl alcohol 7.8 g. of 1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride are obtained.

Quelle