Potassium Carbonate → 2-(4-Bromophenyl)propanenitrile

HRID 76144Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 76144
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][C:7]#[N:8])=[CH:4][CH:3]=1.[CH3:11]OC(=O)OC.C([O-])([O-])=O.[K+].[K+]>CCOC(C)=O>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([CH:6]([CH3:11])[C:7]#[N:8])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 12021Dimethyl CarbonateHCID 27914Benzeneacetonitrile, 4-bromo-

Produkt 1

HCID 107509272-(4-Bromophenyl)propanenitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

An autoclave is charged with 25.0 g (128 mmol) 4-bromobenzylcyanide, 190 mL dimethylcarbonate and 0.900 g (6.51 mmol) K2CO3 and stirred for 16 h at 180° C. Then the reaction mixture is allowed to cool to r.t., the mixture is diluted with EtOAc and washed with water (1×), aq. 10% Na2S2O3 solution (1×) and brine (1×). The organic layer is dried with MgSO4 and the solvent is removed in vacuo. The residue is purified by destillation (bath temperature 204° C., head temperature 153° C.).

Aufarbeitung

  1. temperatureto cool to r.t.
  2. washwashed with water (1×), aq. 10% Na2S2O3 solution (1×) and brine (1×)
  3. dry with materialThe organic layer is dried with MgSO4
  4. customthe solvent is removed in vacuo
  5. customThe residue is purified by destillation (bath temperature 204° C., head temperature 153° C.)

Quellen und Nachweise

ORD-Eintrag
ord-f061d94d1d1049f98482bce5df7fa9f7
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835472B2

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