Hydrochloric Acid → HCID 12888761, Verbindung

HRID 1995277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1995277
[NH2:1][C:2]1[C:6]([C:7]#[N:8])=[CH:5][N:4]([CH3:9])[N:3]=1.F[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N+:17]([O-:19])=[O:18].C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+].Cl>C1(C)C=CC=CC=1.CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-]>[CH3:9][N:4]1[CH:5]=[C:6]([C:7]#[N:8])[C:2]([NH:1][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[N+:17]([O-:19])=[O:18])=[N:3]1

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 738951-Fluoro-2-nitrobenzeneHCID 106542131-Methyl-3-amino-4-cyanopyrazole

Produkt 1

HCID 12888761HCID 12888761, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 21218Trioctylmethylammonium chlorideKatalysatorHCID 1140TolueneLösungsmittel

Versuchsvorschrift

3-Amino-1-methylpyrazole-4-carbonitrile (Helv. Chim. Acta (1959) 42, 763) (7.5 g) and 2-fluoronitrobenzene (8.4 g) were stirred in toluene (120 ml) with Adogen 464 (3.0 g) and potassium carbonate (16.5 g) at 60° C. 50% Sodium hydroxide solution (0.1 ml) was added and the mixture was heated under reflux for 2 hours. The mixture was poured on to dilute hydrochloric acid, extracted, the aqueous layer washed with toluene and the combined extracts washed twice with water. After evaporation the residue was crystallised from ethanol (750 ml) to give the title compound, m.p. 172° C.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. extractionextracted
  4. washthe aqueous layer washed with toluene
  5. washthe combined extracts washed twice with water
  6. customAfter evaporation the residue
  7. customwas crystallised from ethanol (750 ml)

Quellen und Nachweise

ORD-Eintrag
ord-da45cec5632a4c7f8e8ab12dafd9e02e
Quelldatensatz
uspto-grants-1983_09
Patentnummer
US04404137

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