HCID 60046932, Verbindung → HCID 60046926, Verbindung

HRID 1672310Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1672310
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)=[C:7]([N+:12]([O-])=O)[CH:8]=[N:9]2)=[CH:4][CH:3]=1>C1COCC1.CO.[Ni]>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)=[C:7]([NH2:12])[CH:8]=[N:9]2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 1

HCID 60046932HCID 60046932, Verbindung

Produkt 1

HCID 60046926HCID 60046926, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 21899815MeOH tetrahydrofuranLösungsmittel

Versuchsvorschrift

1.3 g (4.09 mmol) (7-chloro-3-nitro-quinolinyl)-(4-fluoro-phenyl)-amine (Example 15c) in 60 ml THF/MeOH 2:1 and 0.6 g Raney-Ni are hydrogenated at rt for 2 h. The reaction solution is filtered on Hyflo® Super Cel diatomaceous earth and is evaporated to dryness. The raw product is dissolved in 30 ml ethyl acetate, and ca. 400 ml hexane are added. The title compound precipitates and is collected by filtration. Drying follows at 65° C. over night. mp: 198-200° C.; MS: 288 (M++1); HPLC: tret=8.38 min (Grad 1).

Aufarbeitung

  1. filtrationThe reaction solution is filtered on Hyflo® Super Cel diatomaceous earth
  2. customis evaporated to dryness
  3. dissolutionThe raw product is dissolved in 30 ml ethyl acetate
  4. additionca. 400 ml hexane are added
  5. customThe title compound precipitates
  6. filtrationis collected by filtration
  7. customDrying
  8. waitfollows at 65° C. over night
  9. customtret=8.38 min (Grad 1)

Quellen und Nachweise

ORD-Eintrag
ord-6f10e01e9c58416595f962f1bd2d17a4
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07998972B2

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