StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Acetic Acid → HCID 25155178, Verbindung

HRID 1158315
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1158315
[CH2:1]([O:17][CH2:18][CH:19]([CH2:29][OH:30])[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH:25]([OH:28])CO)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].C(O)(=O)C>C(O)(C)C.O.C(O)C.C[N+](CC(NN)=O)(C)C.[Cl-]>[CH2:1]([O:17][CH2:18][CH:19]([CH2:29][OH:30])[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH:25]=[O:28])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 2

HCID 176Acetic AcidHCID 25155177HCID 25155177, Verbindung

Produkt 1

HCID 25155178HCID 25155178, VerbindungAusbeute 27 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 67156Girard-T reagentKatalysatorHCID 702EthanolLösungsmittelHCID 962
Water
Lösungsmittel
3×
HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

As depicted in Scheme III, 1-Hexadecyl-2-(5′,6′-dihydroxy-hexanyl)-glycerol (7.84 grams) was dissolved in isopropanol (50 ml) and water (12 ml). NaIO4 (9 grams) was added and the reaction mixture was stirred at room temperature for 3 hours. Water (50 ml) was added and the reaction mixture extracted with chloroform (3×50 ml), dried over anhydrous Na2SO4, filtered and the solvent removed under reduced pressure yielding 5.56 grams. The crude product was dissolved in ethanol (60 ml) and glacial acetic acid (2.3 grams). Girard's reagent T (5.6 grams) was added and the reaction mixture was refluxed for 2 hours. The reaction mixture was cooled in ice-bath, alkaline solution (2.3 grams in 45 ml water) was added and the mixture was extracted with ether (3×25 ml). The etheral phase was washed with water and the water combined with the alkaline phase. The aqueous phase was acidified with concentrated HCl (4.4 ml) and extracted with ether (3×25 ml). Washing with water, saturated aqueous sodium bicarbonate (3×25 ml), water (2×25 ml), drying over anhydrous Na2SO4 and removal of the solvent under reduced pressure gave 1.95 grams (0.0049 mol) of 1-Hexadecyl-2-(5′-oxo-pentanyl)-glycerol (26.9% yield).

Aufarbeitung

  1. extractionthe reaction mixture extracted with chloroform (3×50 ml)
  2. dry with materialdried over anhydrous Na2SO4
  3. filtrationfiltered
  4. customthe solvent removed under reduced pressure
  5. customyielding 5.56 grams
  6. temperaturethe reaction mixture was refluxed for 2 hours
  7. temperatureThe reaction mixture was cooled in ice-bath
  8. extractionthe mixture was extracted with ether (3×25 ml)
  9. washThe etheral phase was washed with water
  10. extractionextracted with ether (3×25 ml)
  11. washWashing with water, saturated aqueous sodium bicarbonate (3×25 ml), water (2×25 ml)
  12. dry with materialdrying over anhydrous Na2SO4 and removal of the solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7a7adaae8972447fb3c4634bca4aeea5
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07807847B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion