Cesium carbonate → HCID 66836638, Verbindung

HRID 1631151Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1631151
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[CH2:10]Cl.C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:18][CH:19]1[CH2:23][CH2:22][CH:21]([CH3:24])[NH:20]1>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[CH2:10][N:20]1[CH:21]([CH3:24])[CH2:22][CH2:23][CH:19]1[CH3:18]

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 960342,5-DimethylpyrrolidineHCID 66836706HCID 66836706, Verbindung

Produkt 1

HCID 66836638HCID 66836638, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

200 mg of 1-bromo-2-chloromethyl-4,5-difluorobenzene are dissolved in 5 ml of acetonitrile. 540 mg of caesium carbonate and 152 μl of 2,5-dimethylpyrrolidine are added, and the mixture is stirred at 80° C. for 16 h. After cooling to 25° C., the mixture is filtered, and the filtrate is evaporated to dryness. The residue is taken up in 5 ml of ethyl acetate, the solution is washed with 5 ml of 2N sodium hydroxide solution, and the combined organic phases are dried over sodium sulfate. After filtration, the filtrate is evaporated to dryness, after which the product is isolated as oil.

Aufarbeitung

  1. temperatureAfter cooling to 25° C.
  2. filtrationthe mixture is filtered
  3. customthe filtrate is evaporated to dryness
  4. washthe solution is washed with 5 ml of 2N sodium hydroxide solution
  5. dry with materialthe combined organic phases are dried over sodium sulfate
  6. filtrationAfter filtration
  7. customthe filtrate is evaporated to dryness
  8. customafter which the product is isolated as oil

Quellen und Nachweise

ORD-Eintrag
ord-ec84a88e47434fcb99fdbd4701c2896a
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08791129B2

Notizen zur Reaktion

Wird geladen…