Potassium Carbonate → HCID 13269152, Verbindung

HRID 542086Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 542086
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=1[OH:18].[Cl:19][C:20]1[CH:25]=[C:24]([N+]([O-])=O)[CH:23]=[C:22]([Cl:29])[N:21]=1>>[Cl:19][C:20]1[CH:25]=[C:24]([O:18][C:9]2[CH:10]=[CH:11][C:12]([C:14]([F:16])([F:17])[F:15])=[CH:13][C:8]=2[Cl:7])[CH:23]=[C:22]([Cl:29])[N:21]=1

Komponenten

4

Edukt 3

HCID 11430Potassium CarbonateHCID 27366032-Chloro-4-(trifluoromethyl)phenolHCID 38410702,6-Dichloro-4-nitropyridine

Produkt 1

HCID 13269152HCID 13269152, Verbindung

Versuchsvorschrift

16.5 gm (0.12 mol) of potassium carbonate were added in portions to an ice-cooled and stirred suspension of 19.65 gm (0.1 mol) of 2-chloro-4-trifluoromethyl-phenol and 19.29 gm (0.1 mol) of 2,6-dichloro-4-nitro-pyridine. The resulting mixture was stirred for 2 hours at room temperature, and was then stirred into 250 ml of ice water. An oil separated out, which crystallized after some time. The crystalline product was collected by suction filtration, washed with water and dissolved in chloroform. The resulting solution was shaken with water, and the organic phase was separated, dried with sodium sulfate and evaporated to dryness. 25.3 gm (75% of theory) of the title compound were obtained as a colorless substance having a melting point of 66° C.

Aufarbeitung

  1. temperaturecooled
  2. stirringThe resulting mixture was stirred for 2 hours at room temperature
  3. customAn oil separated out
  4. customwhich crystallized after some time
  5. filtrationThe crystalline product was collected by suction filtration
  6. washwashed with water
  7. dissolutiondissolved in chloroform
  8. stirringThe resulting solution was shaken with water
  9. customthe organic phase was separated
  10. dry with materialdried with sodium sulfate
  11. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-9cd8efd21407499e894eb4a058c5a3c6
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04655824

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