Reaktionsgleichung
[C:1](Cl)(=[O:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].ON[N:18]=[CH:19][CH:20]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)[C:21]([NH:23][C:24]1[C:29]([O:30][CH3:31])=[CH:28][C:27]([O:32][CH3:33])=[CH:26][C:25]=1[O:34][CH3:35])=[O:22].CC[N:44](C(C)C)C(C)C>C1COCC1>[CH2:2]([C:1]1[O:14][N:44]=[C:19]([CH:20]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[C:21]([NH:23][C:24]2[C:29]([O:30][CH3:31])=[CH:28][C:27]([O:32][CH3:33])=[CH:26][C:25]=2[O:34][CH3:35])=[O:22])[N:18]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
Tridecanoyl chloride (15.08 g, 0.061 mol) was added to a mixture of α-[(hydroxyamino)iminomethyl]-N-(2,4,6-trimethoxyphenyl)-benzene acetamide (19.8 g, 0.055 mol), Hunig's base (10.6 mL, 0.061 mol), and THF (200 mL). The mixture was stirred in THF at room temperature for 2 hours, then concentrated in vacuo and dissolved in glacial acetic acid (50 mL) and refluxed for 2 hours, then concentrated in vacuo, azeotroped with toluene (2×250 mL), and columned on silica gel eluting with 35% ethyl acetate in hexanes to yield a white solid (12.1 g, 62%). %(found): C, 68.93; H, 7.96; N, 7.54.
Aufarbeitung
- concentrationconcentrated in vacuo
- dissolutiondissolved in glacial acetic acid (50 mL)
- temperaturerefluxed for 2 hours
- concentrationconcentrated in vacuo
- customazeotroped with toluene (2×250 mL)
Quellen und Nachweise
- ORD-Eintrag
- ord-a322a9773da24e4bb2aab4466ab1a1dc
- Quelldatensatz
- uspto-grants-1997_07
- Patentnummer
- US05646170
Verknüpfte Notizen
Wird geladen…