HCID 22649188, Verbindung → HCID 22649208, Verbindung

HRID 1782079Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1782079
[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-(6,7dimethoxyquinazolin-4-yl)-3-(2-nitrophenyl)urea (0.18 g), 10% palladium 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) 3.95-3.95 (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-e167641bb4ba41f38ad99a7e66918a01
Quelldatensatz
uspto-grants-2009_03
Patentnummer
US07498335B2

Notizen zur Reaktion

Wird geladen…