HCID 22649188, Verbindung → HCID 22649208, Verbindung

HRID 393250Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 393250
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][N:7]=[C:6]2[NH:15][C:16]([NH:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N+:25]([O-])=O)=[O:17]>[Pd].CN(C=O)C>[NH2:25][C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=1[NH:18][C:16]([NH:15][C:6]1[C:5]2[C:10](=[CH:11][C:12]([O:13][CH3:14])=[C:3]([O:2][CH3:1])[CH:4]=2)[N:9]=[CH:8][N:7]=1)=[O:17]

Komponenten

4

Edukt 1

HCID 22649188HCID 22649188, Verbindung

Produkt 1

HCID 22649208HCID 22649208, VerbindungAusbeute 82,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 1-(6,7-dimethoxyquinazolin-4-yl)-3-(2-nitrophenyl)urea (0.18 g), 10% palladium-on-charcoal catalyst (0.023 g) and DMF (10 ml) was stirred at ambient temperature under an atmosphere of hydrogen for 16 hours. The reaction mixture was filtered and the filtrate was evaporated. The resultant gum was triturated under ethyl acetate and there was thus obtained the title compound as a solid (0.137 g); NMR Spectrum: (DMSOd6) 3.85-3.95 (br s, 8H), 6.63 (t, 1H), 6.81 (d, 1H), 6.91 (t, 1H), 7.25 (s, 1H), 7.47 (d, 1H), 8.05 (s, 1H), 8.64 (s, 1H), 10.28 (br s, 1H), 11.74 (br s, 1H); Mass Spectrum: M+H+ 340.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate was evaporated
  3. customThe resultant gum was triturated under ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-7ef714cbafa84f3ea5e084763775662e
Quelldatensatz
uspto-grants-2004_10
Patentnummer
US06806274B1

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