Sodium Cyanide → HCID 13654087, Verbindung

HRID 280451Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 280451
Cl[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[C:14]([F:17])([F:16])[F:15])[N:5]=[CH:4][C:3]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19].[C-:23]#[N:24].[Na+]>CN(C)C=O>[C:23]([C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[C:14]([F:17])([F:16])[F:15])[N:5]=[CH:4][C:3]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19])#[N:24]

Komponenten

4

Edukt 2

HCID 8929Sodium CyanideHCID 13654085HCID 13654085, Verbindung

Produkt 1

HCID 13654087HCID 13654087, VerbindungAusbeute 32,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 3.15 g of 5-chloro-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester and 1.1 g of sodium cyanide in 25 ml of dimethylformamide was heated at approximately 100° C. for four and one-half hours. The reaction mixture also contained approximately 3 g of molecular sieve to insure dryness. The reaction mixture was cooled and poured into approximately 300 ml of ice water. The precipitated solid was collected by filtration and recrystallized from ethanol (charcoal) to provide 1 g of 5-cyano-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester. MP=70°-72° C.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. filtrationThe precipitated solid was collected by filtration
  3. customrecrystallized from ethanol (charcoal)

Quellen und Nachweise

ORD-Eintrag
ord-34d8f69ec7724bc3a1ee3a54570d3542
Quelldatensatz
uspto-grants-1986_05
Patentnummer
US04589905

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