Reaktion #530710

ord-9c1bba6f9a0740a2934ade15aec69a43

Reaktionsgleichung

[H][H]
hydrogen
O=C(CCc1ccccc1)CCc1ccccc1
1,5-di-(phenyl)-3-pentanone
NCC(O)CN
1,3-diamino-2-hydroxypropane
[H][H]
hydrogen
NCC(O)CNC(CCc1ccccc1)CCc1ccccc1
1-amino-3-[1,5-di-(phenyl)-3-pentylamino]-2-propanol

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

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-(phenyl)-3-pentanone (9.5 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 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-(phenyl)-3-pentylamino]-2-propanol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04260760uspto-grants-1981_04