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Dicyclohexylcarbodiimide → Diisopropyl ether ethanol

HRID 1939891
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1939891
[OH:1][C:2]1[C:10]2N=NNC=2C=C[CH:3]=1.[CH:11]1(N=C=NC2CCCCC2)[CH2:16]CCC[CH2:12]1>CN(C)C=O>[CH2:2]([OH:1])[CH3:3].[CH:11]([O:1][CH:2]([CH3:3])[CH3:10])([CH3:16])[CH3:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 10868DicyclohexylcarbodiimideHCID 178418300HCID 178418300, Verbindung

Produkt 1

HCID 23358034Diisopropyl ether ethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

Then, at 20° C., 18.3 g (0.12 mol) of hydroxybenzotriazole (HOBT), 23.7 g (0.109 mol) of N-4-trifluoromethylbenzyl-N-n-propylamine and 25.6 g (0.125 mol) of dicyclohexyl-carbodiimide (DCCI) and a further 250 ml of dimethylformamide (DMF) were added. The mixture was left to react for 24 hours. It was then cooled to 5° C. and filtered. 500 ml of water were added to the filtrate and it was extracted with ethyl acetate. The combined organic phases were washed with water and saturated sodium hydrogen carbonate solution, dried with magnesium sulphate and filtered over kieselguhr/char-coal. After working up in the usual way, 50 g of colourless crystals of the title compound are obtained by crystallisation from ethanol/diisopropylether (1:1). The 3H-PAF-receptor bonding--determined using human thrombocytes--is Ki =1.8 nMol/liter. (The method used is described for example in European Patent Application 368 175).

Aufarbeitung

  1. waitThe mixture was left
  2. customto react for 24 hours
  3. filtrationfiltered
  4. addition500 ml of water were added to the filtrate and it
  5. extractionwas extracted with ethyl acetate
  6. washThe combined organic phases were washed with water and saturated sodium hydrogen carbonate solution
  7. dry with materialdried with magnesium sulphate
  8. filtrationfiltered over kieselguhr/char-coal

Quellen und Nachweise

ORD-Eintrag
ord-ca2cdcfad3ee4f1285418e0b70278f44
Quelldatensatz
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05698552

Notizen zur Reaktion

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