Reaktionsgleichung
[CH3:1][N:2]([CH:4]=[C:5]1[C:11](=O)[C:10]2[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=2[N:8]([C:17](=[O:27])[C:18]2[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=2)[CH2:7][CH2:6]1)C.C[NH:29]N>CO>[CH3:1][N:2]1[CH:4]=[C:5]2[CH2:6][CH2:7][N:8]([C:17](=[O:27])[C:18]3[CH:19]=[CH:20][C:21]([N+:24]([O-:26])=[O:25])=[CH:22][CH:23]=3)[C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11]2=[N:29]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 0.150 g of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 44 μl of methylhydrazine in 5 ml of methyl alcohol is heated at reflux for 18 hours. A precipitate forms on standing. The volatiles are evaporated to a residue which is purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride. The product fractions are combined and the volatiles evaporated to a residue which is dissolved in chloroform-methanol, filtered through glass wool and the filtrate evaporated in vacuo to give 0.110 g of the desired product as pale yellow crystals.
Aufarbeitung
- temperatureat reflux for 18 hours
- customThe volatiles are evaporated to a residue which
- customis purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride
- customthe volatiles evaporated to a residue which
- dissolutionis dissolved in chloroform-methanol
- filtrationfiltered through glass wool
- customthe filtrate evaporated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-f2441699a4154e82a18ddbb00b69d577
- Quelldatensatz
- uspto-grants-1998_11
- Patentnummer
- US05834461
Verknüpfte Notizen
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