Reaktionsgleichung
[N+:1]([C:4]1[CH:23]=[CH:22][C:7]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[C:14](=[O:21])[CH2:13][CH2:12][CH2:11]2)=[O:9])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(O[CH:29](N(C)C)[N:30]([CH3:32])[CH3:31])(C)(C)C>>[CH3:29][N:30]([CH:32]=[C:13]1[C:14](=[O:21])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[N:10]([C:8](=[O:9])[C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:23][CH:22]=2)[CH2:11][CH2:12]1)[CH3:31]Komponenten
Versuchsvorschrift
A mixture of 1.35 g of 1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 15 ml of tert-butoxy-bis(dimethylamino)methane is heated for on a steam bath for 2 hours. The volatiles are evaporated in vacuo to a residue which is stirred with ether and filtered. The cake is washed with ether and the combined filtrates evaporated in vacuo to a residue which is dissolved in 30% ethyl acetate in methylene chloride and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated in vacuo to a residue which is dissolved in 30% ethyl acetate in methylene chloride and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated in vacuo to a residue to give 1.60 g of yellow crystalline product, m.p. 180°-183° C.
Aufarbeitung
- temperatureis heated for on a steam bath for 2 hours
- customThe volatiles are evaporated in vacuo to a residue which
- filtrationfiltered
- washThe cake is washed with ether
- customthe combined filtrates evaporated in vacuo to a residue which
- dissolutionis dissolved in 30% ethyl acetate in methylene chloride
- customThe filtrate is evaporated in vacuo to a residue which
- dissolutionis dissolved in 30% ethyl acetate in methylene chloride
- customThe filtrate is evaporated in vacuo to a residue
Quellen und Nachweise
- ORD-Eintrag
- ord-6530b21b14864ff38f3f266efa748f7a
- Quelldatensatz
- uspto-grants-1998_11
- Patentnummer
- US05834461
Verknüpfte Notizen
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