Reaktion #54278

Reaktionsgleichung

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

isopropylamine

→

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

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Sonstigethe ethanol and excess amine are removed by distillation under reduced pressure
3. 3
   ExtraktionThe residue is extracted with 100 ml
4. 4
   Waschenof 1N HCl and the extract is washed twice with 50 ml
5. 5
   ExtraktionThe hydrochloric acid extract
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
    Filtrationis filtered
11. 11
    Sonstigedried
12. 12
    SonstigeUpon recrystallization of the crude crystals from isopropyl alcohol, 6.4 g

Vorschrift

20.5 g. of 1-(3,4-methylenedioxyphenyl)-2-chloroethanol are mixed with 30 g. of isopropylamine and 100 ml. of ethanol and the mixture is refluxed for 8 hours. After cooling, the ethanol and excess amine are removed by distillation under reduced pressure. The residue is extracted with 100 ml. of 1N HCl and the extract is washed twice with 50 ml. of ether. The hydrochloric acid extract 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. The crystalline hydrochloride settles out of solution and is filtered and dried. Upon recrystallization of the crude crystals from isopropyl alcohol, 6.4 g. of 1 -(3,4-methylenedioxyphenyl)-2-isopropylaminoethanol hydrochloride are obtained.

Quelle