Reaktion #95398

Reaktionsgleichung

1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane

1-ethinyl-cyclohexyl-amine

→

1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-3-(1-ethinyl-cyclohexylamino)-2-propanol

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for one hour
2. 2
   workup.DISTILLATIONThe solvent was then distilled off
3. 3
   ExtraktionAfter extraction with ethyl acetate the aqueous phase
4. 4
   workup.ADDITIONby addition of NaOH, whereby basic components
5. 5
   Sonstigeprecipitated in oily form
6. 6
   Waschenthe organic phase was washed with water
7. 7
   Trocknendried over MgSO4
8. 8
   Sonstigeevaporated
9. 9
   Sonstigethe solid residue was recrystallized twice from acetonitrile

Vorschrift

7.8 gm (0.03 mol) of 1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane were dissolved in 80 ml of ethanol, and after addition of 7.5 gm (0.06 mol) of 1-ethinyl-cyclohexyl-amine the mixture was refluxed for one hour. The solvent was then distilled off, and the residue was acidified with dilute HCl. After extraction with ethyl acetate the aqueous phase was made alkaline by addition of NaOH, whereby basic components precipitated in oily form. They were taken up in ethyl acetate, the organic phase was washed with water, dried over MgSO4, evaporated and the solid residue was recrystallized twice from acetonitrile.

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