Potassium Carbonate → HCID 21938673, Verbindung

HRID 1242251Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1242251
I[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[C:11]=1[NH2:12].C(=O)([O-])[O-].[K+].[K+]>C1(C)C(C)=CC=CC=1.CCCCCCC.[Cu]>[Cl:9][C:10]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[C:11]=1[NH:12][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1

Komponenten

7

Edukt 3

HCID 11430Potassium CarbonateHCID 122074-IodotolueneHCID 27340832-Chloro-4,6-difluoroaniline

Produkt 1

HCID 21938673HCID 21938673, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23978CopperKatalysatorHCID 7237O-XyleneLösungsmittelHCID 8900HeptaneLösungsmittel

Versuchsvorschrift

A mixture of 4-iodotoluene (210 g, 0.96 mol), 2-chloro-4,6-difluoroaniline (204 g, 1.25 mol), copper powder (36 g, 0.57 mol), cuprous iodide (130 g, 0.68 mol), and potassium carbonate (118 g, 0.86 mol) in 500 ml of xylene is stirred vigorously and heated to reflux in a flask fitted with a Dean-Stark trap for 26 hours. After cooling to room temperature, the solids are filtered off, and the filter cake is washed with 100 ml of xylene. The solvents are evaporated under reduced pressure to give an oil which is dissolved in a mixture of 50 g of silica gel in 750 ml of heptane. The solids are filtered off and the solvents are evaporated under reduced pressure to give N-(2′-chloro-4′,6′-difluorophenyl)-4-methylaniline as an oil.

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux in a flask
  3. customfitted with a Dean-Stark trap for 26 hours
  4. filtrationthe solids are filtered off
  5. washthe filter cake is washed with 100 ml of xylene
  6. customThe solvents are evaporated under reduced pressure
  7. customto give an oil which
  8. filtrationThe solids are filtered off
  9. customthe solvents are evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2c026e4d692947e2a345b16dae5aa2ae
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07115662B2

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