4-Fluoroaniline → HCID 60046932, Verbindung

HRID 1672309Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1672309
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:12])=[CH:9][CH:10]=2)[N:5]=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].[F:16][C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=1>O>[Cl:12][C:8]1[CH:7]=[C:6]2[C:11]([C:2]([NH:21][C:20]3[CH:22]=[CH:23][C:17]([F:16])=[CH:18][CH:19]=3)=[C:3]([N+:13]([O-:15])=[O:14])[CH:4]=[N:5]2)=[CH:10][CH:9]=1

Komponenten

4

Edukt 2

HCID 97314-FluoroanilineHCID 534398754,7-Dichloro-3-nitroquinoline

Produkt 1

HCID 60046932HCID 60046932, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

1.3 g (5.3 mmol) 4,7-dichloro-3-nitro-quinoline (Example 15b) and 0.525 g (5.3 mmol) 4-fluoroaniline are stirred at rt for 1 h. The reaction mixture is poured into 150 ml of water, and the resulting crystals are filtered off. After washing with water, the solid is dissolved in ca. 170 ml of ethanol and then concentrated to ca. 30 ml. The solution is cooled in ice-water. The crystals which precipitate are filtered off and dried overnight at 70° C. (high vacuum). mp: 198-200° C.; MS: 318 (M++1); HPLC: tret=10.92 min (Grad 1).

Aufarbeitung

  1. filtrationthe resulting crystals are filtered off
  2. washAfter washing with water
  3. dissolutionthe solid is dissolved in ca. 170 ml of ethanol
  4. concentrationconcentrated to ca. 30 ml
  5. temperatureThe solution is cooled in ice-water
  6. filtrationThe crystals which precipitate are filtered off
  7. customdried overnight at 70° C. (high vacuum)
  8. customtret=10.92 min (Grad 1)

Quellen und Nachweise

ORD-Eintrag
ord-ace51838c99e490f8f2c6e54d9902c88
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07998972B2

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