Reaktion #953897

Reaktionsgleichung

hydrogen

1,5-di-(3,3-dimethylbicyclo[2.2.2]oct-2-yl)-3-pentanone

1,3-diamino-2-hydroxypropane

hydrogen

→

1-amino-3-[1,5-di-(3,3-dimethylbicyclo[2.2.2]oct-2-yl)-3-pentylamino]-2-propanol

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting mixture is then heated
2. 2
   Temperaturat reflux for about two hours
3. 3
   Temperaturto cool
4. 4
   FiltrationThe mixture is then filtered from the catalyst
5. 5
   Einengenconcentrated in vacuo
6. 6
   Sonstigeto remove the ethanol
7. 7
   Waschenwashed with water
8. 8
   Trocknendried over sodium sulfate
9. 9
   Filtrationfiltered
10. 10
    Einengenconcentrated in vacuo

Vorschrift

A solution of 1,5-di-(3,3-dimethylbicyclo[2.2.2]oct-2-yl)-3-pentanone (14.8 g., 0.04 mole) in 50 cc of anhydrous ethanol is added dropwise over about 20 minutes to a stirred solution of 1,3-diamino-2-hydroxypropane (25 g., 0.27 mole) in 200 cc of ethanol. The resulting mixture is then heated at reflux for about two hours, allowed to cool, 1.0 g. platinum oxide added, and the mixture reduced under a 40 psi hydrogen atmosphere until hydrogen uptake ceases. The mixture is then filtered from the catalyst, concentrated in vacuo to remove the ethanol, the oily residue taken up in ether (250 cc.), washed with water, dried over sodium sulfate, filtered and concentrated in vacuo to yield the product 1-amino-3-[1,5-di-(3,3-dimethylbicyclo[2.2.2]oct-2-yl)-3-pentylamino]-2-propanol.

Quelle