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

2-(4-Bromo-2,6-dimethylphenyl)-3-methoxy-cyclopent-2-enone → 2-(2,6-Dimethyl-4-prop-1-ynylphenyl)-3-methoxycyclopent-2-enone

HRID 514191
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 514191
[C:1]([Mg]Br)#[C:2][CH3:3].Br[C:7]1[CH:12]=[C:11]([CH3:13])[C:10]([C:14]2[C:15](=[O:21])[CH2:16][CH2:17][C:18]=2[O:19][CH3:20])=[C:9]([CH3:22])[CH:8]=1>O1CCCC1.[Br-].[Zn+2].[Br-].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH3:3][C:2]1[CH:1]=[C:7]([C:12]#[C:11][CH3:13])[CH:8]=[C:9]([CH3:22])[C:10]=1[C:14]1[C:15](=[O:21])[CH2:16][CH2:17][C:18]=1[O:19][CH3:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 668681542-(4-Bromo-2,6-dimethylphenyl)-3-methoxy-cyclopent-2-enoneHCID 178419101HCID 178419101, Verbindung

Produkt 1

HCID 896009282-(2,6-Dimethyl-4-prop-1-ynylphenyl)-3-methoxycyclopent-2-enone

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 10421208Zinc bromideKatalysator
HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
Katalysator
HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of anhydrous zinc bromide (1.41 g, 6.3 mmol) in anhydrous tetrahydrofuran (8.0 ml) under nitrogen at 0°C., is added propynylmagnesium bromide (15.7 ml, 6.3 mmol, 0.4 M solution in tetrahydrofuran) dropwise. The reaction mixture is then allowed to warm to room temperature and stir for 10 minutes, then cooled again to 0°C. To this mixture is then added [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.102 g, 0.13 mmol), followed by a solution of 2-(4-bromo-2,6-dimethylphenyl)-3-methoxycyclopent-2-enone (0.370 g, 1.25 mmol) in anhydrous tetrahydrofuran (4.0 ml). The reaction mixture is heated at reflux for 4.5 hours, then allowed to cool to room temperature followed by quenching with saturated aqueous ammonium chloride (10 ml). Ethyl acetate is added, and the mixture is filtered through a bed of diatomaceous earth and the phases separated. The aqueous phase is extracted again with ethyl acetate (×3) and combined organics are washed with brine, dried over magnesium sulfate, filtered and the filtrate concentrated in vacuo. The residue is purified by flash column chromatography (ethyl acetate and isohexane as eluant) to afford 2-(2,6-dimethyl-4-prop-1-ynylphenyl)-3-methoxycyclopent-2-enone.

Aufarbeitung

  1. temperaturecooled again to 0°C
  2. temperatureThe reaction mixture is heated
  3. temperatureat reflux for 4.5 hours
  4. temperatureto cool to room temperature
  5. customby quenching with saturated aqueous ammonium chloride (10 ml)
  6. additionEthyl acetate is added
  7. filtrationthe mixture is filtered through a bed of diatomaceous earth
  8. customthe phases separated
  9. extractionThe aqueous phase is extracted again with ethyl acetate (×3)
  10. washcombined organics are washed with brine
  11. dry with materialdried over magnesium sulfate
  12. filtrationfiltered
  13. concentrationthe filtrate concentrated in vacuo
  14. customThe residue is purified by flash column chromatography (ethyl acetate and isohexane as eluant)

Quellen und Nachweise

ORD-Eintrag
ord-5bd59fc45cb84060ad2314942be37297
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09107415B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion