Reaktionsgleichung
[C:1](Cl)(=[O:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[C:12]([C:16]1[CH:17]=[C:18]([CH2:27][CH2:28][C:29]([NH:31][NH2:32])=[O:30])[CH:19]=[C:20]([C:23]([CH3:26])([CH3:25])[CH3:24])[C:21]=1[OH:22])([CH3:15])([CH3:14])[CH3:13]>O>[C:1]([NH:32][NH:31][C:29](=[O:30])[CH2:28][CH2:27][C:18]1[CH:19]=[C:20]([C:23]([CH3:24])([CH3:26])[CH3:25])[C:21]([OH:22])=[C:16]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:17]=1)(=[O:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1Komponenten
Versuchsvorschrift
To 50 ml of N-dimethylacetamide were added 2.30 g of cinnamoyl chloride and 4.04 g of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionylhydrazine, and the resulting mixture was stirred at 30° - 35° C for 3 hours. The reaction mixture was then poured into 2 liters of water, and the produced precipitate was collected by filtration and washed with water. The so obtained precipitate was then recrystallized twice from a mixture of ethanol (first grade) and water (1 : 1, volume ratio) and dried under reduced pressure to yield 4.1 g of N-cinnamoyl-N'-{β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl}-hydrazine as white crystals, m.p. 224.5° - 225.0° C. Analysis for C26H34N2O8 : C, 73.90%, H, 8.11%; N, 6.63%, Found: C, 73.91%; H, 7.90%; N, 6.51%.
Aufarbeitung
- filtrationthe produced precipitate was collected by filtration
- washwashed with water
- customThe so obtained precipitate
- customwas then recrystallized twice from a mixture of ethanol (first grade) and water (1 : 1, volume ratio)
- customdried under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-8e55ecb57f594a1b87a5a2ce4c60b3a7
- Quelldatensatz
- uspto-grants-1977_10
- Patentnummer
- US04052362
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