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4-Amino-2-(trifluoromethyl)benzonitrile → HCID 11246104, Verbindung

HRID 982665
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 982665
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]1[C:8](=[O:14])O[C:10](=[O:13])[C:11]=1[CH3:12].[NH2:15][C:16]1[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[C:18]([C:24]([F:27])([F:26])[F:25])[CH:17]=1>C(O)C>[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]1[C:8](=[O:14])[N:15]([C:16]2[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[C:18]([C:24]([F:25])([F:26])[F:27])[CH:17]=2)[C:10](=[O:13])[C:11]=1[CH3:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 5221704-Amino-2-(trifluoromethyl)benzonitrileHCID 113789433-(5-Chloropentyl)-4-methyl-2,5-furandione

Produkt 1

HCID 11246104HCID 11246104, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of 9.46 g of 3-(5-chloropentyl)-4-methyl-2,5-furandione and 8.13 g of 4-amino-2-(trifluoromethyl)benzonitrile in 22 ml of ethanol was mixed under a nitrogen atmosphere with 2.5 g of an activated molecular sieve (0.3 nm), and it was stirred for 2 days at 90° C. For working-up, the molecular sieve was filtered off after cooling, washed with ethanol, and the combined ethanol solutions were concentrated by evaporation. The residue was taken up in ethyl acetate and washed with water as well as saturated sodium chloride solution. After drying on sodium sulfate and concentration by evaporation, it was chromatographed on silica gel with ethyl acetate/hexane/toluene, and 11.69 g of the title compound was thus obtained as a white solid.

Aufarbeitung

  1. additionwas mixed under a nitrogen atmosphere with 2.5 g of an activated molecular sieve (0.3 nm), and it
  2. filtrationthe molecular sieve was filtered off
  3. temperatureafter cooling
  4. washwashed with ethanol
  5. concentrationthe combined ethanol solutions were concentrated by evaporation
  6. washwashed with water as well as saturated sodium chloride solution
  7. customAfter drying on sodium sulfate and concentration by evaporation, it
  8. customwas chromatographed on silica gel with ethyl acetate/hexane/toluene, and 11.69 g of the title compound
  9. customwas thus obtained as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-4a049e2a72a5434eb0e8de77a4fe005e
Quelldatensatz
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06861432B2

Notizen zur Reaktion

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