Chloroform → HCID 21199122, Verbindung

HRID 1066282

Reaktionsgleichung

Reaktionsgleichung von HRID 1066282
[CH3:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:3]=1[C:4]#[N:5].[Br:11]Br.C(Cl)(Cl)Cl.[Al+3].[Cl-].[Cl-].[Cl-]>O>[Br:11][C:9]1[C:2]([CH3:1])=[C:3]([C:6]([CH3:10])=[CH:7][CH:8]=1)[C:4]#[N:5]

Komponenten

6

Edukt 4

HCID 6212ChloroformHCID 24408BromineHCID 810572,6-DimethylbenzonitrileHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 21199122HCID 21199122, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 2,6-dimethylbenzonitrile (5.0 g, 38.0 mmol), bromine (1.9 ml, 38.0 mmol) and chloroform (10 ml) is stirred at room temperature for 24 hours and subsequently heated to 60° C. for 6 hours. Upon cooling down to 0° C., 10 g of AlCl3 are added and the mixture is stirred for 4 hours at 0° C. The reaction mixture is poured into water and extracted with toluene. The organic phase is separated and concentrated and the residue is purified by column chromatography yielding the pure product as brown crystals, 6.2 g, mp. 60° C.

Aufarbeitung

  1. temperaturesubsequently heated to 60° C. for 6 hours
  2. temperatureUpon cooling down to 0° C.
  3. stirringthe mixture is stirred for 4 hours at 0° C
  4. extractionextracted with toluene
  5. customThe organic phase is separated
  6. concentrationconcentrated
  7. customthe residue is purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-c743b4deb59541ecad943013fd7950f7
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06242498B1

Verknüpfte Notizen

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