Reaktionsgleichung
[CH3:1][Si:2]([CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[CH:9][CH:8]=1)([CH3:4])[CH3:3].[C:15]([NH2:21])(=[O:20])[CH2:16][C:17]([NH2:19])=[O:18].N1CCCCC1.C(O)(=O)C>C1(C)C=CC=CC=1.O>[CH3:1][Si:2]([CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=[C:16]([C:15]([NH2:21])=[O:20])[C:17]([NH2:19])=[O:18])=[CH:9][CH:8]=1)([CH3:4])[CH3:3]Komponenten
7
Versuchsvorschrift
4-(Trimethylsilanylmethoxy)benzaldehyde (obtained in step 1 of Example 1) (10.4 g, 0.005 mol) and malonamide (5.5 g, 0.055 mol) in 20 ml of dry toluene in the presence of 0.5 ml of piperidine and 0.3 g of acetic acid are refluxed for 3 hours in a reactor equipped with Dean-Stark apparatus. The water formed is removed azeotropically. The mixture is cooled and the organic phase is washed twice with water. The organic phase is dried over sodium sulfate and filtered, and the solvent is evaporated off under vacuum. After recrystallization from ethanol, 7.2 g (yield: 49%) of the derivative of Example 10 are obtained in the form of an off-white powder:
Aufarbeitung
- customequipped with Dean-Stark apparatus
- customis removed azeotropically
- temperatureThe mixture is cooled
- washthe organic phase is washed twice with water
- dry with materialThe organic phase is dried over sodium sulfate
- filtrationfiltered
- customthe solvent is evaporated off under vacuum
- customAfter recrystallization from ethanol, 7.2 g (yield: 49%) of the derivative of Example 10
- customare obtained in the form of an off-white powder
Quellen und Nachweise
- ORD-Eintrag
- ord-cc4c636fed4448b8bbc95fc511865ee1
- Quelldatensatz
- uspto-grants-2008_04
- Patentnummer
- US07354571B2
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