Water → HCID 816842, Verbindung

HRID 911712Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 911712
[C:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1)#[N:2].[Cl-].[Cl-].[Cl-].[Al+3].O>C1(C)C=CC=CC=1.C(OCC)C>[CH3:1][C:3]1[CH:11]=[CH:10][C:6]([C:7]([C:6]2[CH:10]=[CH:11][C:3]([C:1]#[N:2])=[CH:4][CH:5]=2)=[O:8])=[CH:5][CH:4]=1

Komponenten

6

Edukt 3

HCID 962WaterHCID 801724-Cyanobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 816842HCID 816842, VerbindungAusbeute 97,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Suspend 4-cyanobenzoyl chloride (2.0 g, 12 mmol) in anhydrous toluene (30 mL). Add aluminum trichloride (2.4 g, 18 mmol) in three portions and stir the reaction mixture at ambient temperature overnight. Cool to 0° C., add carefully water and extract the mixture twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to give a solid. Suspend the solid in diethyl ether and filter to obtain the desired intermediate (1.30 g, 49%) that was used without any further purification. GC-MS m/z: 221 (Me).

Aufarbeitung

  1. extractionextract the mixture twice with EtOAc
  2. dry with materialDry the combined organic extracts over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate in vacuo
  5. customto give a solid
  6. filtrationfilter

Quellen und Nachweise

ORD-Eintrag
ord-aa71689b27824ebcbec2471aa4b7a42f
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08022062B2

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