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

Acetic Anhydride → HCID 22116935, Verbindung

HRID 1779472
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1779472
[CH3:1][C:2]1([CH3:24])[C:6](=[O:7])[N:5]([C:8]2[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([C:16]([F:19])([F:18])[F:17])[CH:9]=2)[C:4](=[O:20])[N:3]1[CH2:21][CH2:22][OH:23].[C:25](OC(=O)C)(=[O:27])[CH3:26].C(=O)(O)[O-].[Na+]>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[C:25]([O:23][CH2:22][CH2:21][N:3]1[C:2]([CH3:24])([CH3:1])[C:6](=[O:7])[N:5]([C:8]2[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([C:16]([F:17])([F:18])[F:19])[CH:9]=2)[C:4]1=[O:20])(=[O:27])[CH3:26]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 11244736HCID 11244736, Verbindung

Produkt 1

HCID 22116935HCID 22116935, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 1049
Pyridine
Lösungsmittel

Versuchsvorschrift

A mixture of 215 mg of the product of Example 43, 15 mg of 4-dimethylamino-pyridine, 1 ml of pyridine and 0.5 ml of acetic acid anhydride was stirred at room temperature for 30 minutes and was then poured into 20 ml of a saturated aqueous sodium bicarbonate solution. After stirring for 20 minutes, the mixture was extracted with ethyl acetate. The organic phase was washed with water and evaporated to dryness and the pyridine and residual acetic acid were distilled. The residue was chromatographed on silica and eluted with a 65-35 methylene chloride-ethyl acetate mixture. The residue with a Rf=0.35 was taken up in isopropanol, partially concentrated, iced and vacuum filtered to obtain after drying, 210 mg of the desired product melting at 99° C. to 100° C.

Aufarbeitung

  1. stirringAfter stirring for 20 minutes
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic phase was washed with water
  4. customevaporated to dryness
  5. distillationthe pyridine and residual acetic acid were distilled
  6. customThe residue was chromatographed on silica
  7. washeluted with a 65-35 methylene chloride-ethyl acetate mixture
  8. concentrationpartially concentrated
  9. filtrationiced and vacuum filtered
  10. customto obtain
  11. customafter drying

Quellen und Nachweise

ORD-Eintrag
ord-4935f2a714d24a27b72546f985fe07de
Quelldatensatz
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05627201

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion