Water → 6-[2-(4-Methoxy-2-nitrophenyl)hydrazinylidene]-3-[3-(trimethylsilyl)propoxy]cyclohexa-2,4-dien-1-one
Reaktionsgleichung
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]=[N:10][C:11]2[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:12]=2[OH:18])=[C:5]([N+:19]([O-:21])=[O:20])[CH:4]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:29][CH2:30][CH2:31][Si:32]([CH3:35])([CH3:34])[CH3:33].O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]=[N:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:29][CH2:30][CH2:31][Si:32]([CH3:35])([CH3:34])[CH3:33])=[CH:13][C:12]=2[OH:18])=[C:5]([N+:19]([O-:21])=[O:20])[CH:4]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 75 °C
Versuchsvorschrift
A mixture of 4-(4-methoxy-2-nitrophenylazo)benzene-1,3-diol (2.5 g, i.e. 0.0086 mol) and potassium carbonate (1.24 g) in 30 ml of dimethylformamide was brought to 70-75° C. 3-Chloropropyltrimethylsilane (1.24 g, i.e. 0.0086 mol) was added thereto over 20 minutes. The mixture was stirred at 75° C. for 6 hours. The reaction mixture was then poured into 50 ml of water and extracted with diisopropyl ether. The organic phase was dried, concentrated and purified by column chromatography (eluent: 50/50 heptane/CH2Cl2) to give compound (9) in the form of a red powder.
Aufarbeitung
- customwas brought to 70-75° C
- extractionextracted with diisopropyl ether
- customThe organic phase was dried
- concentrationconcentrated
- custompurified by column chromatography (eluent: 50/50 heptane/CH2Cl2)
Quellen und Nachweise
- ORD-Eintrag
- ord-a1a0dcf316584d059517a64345bc6920
- Quelldatensatz
- uspto-grants-2000_02
- Patentnummer
- US06027537
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