Reaktionsgleichung
[CH3:1][N:2]([C:8]1[CH:17]=[CH:16][C:15]2[C:10](=[C:11]([CH2:18][CH2:19][NH:20][C:21](=[O:29])[CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:12]=[CH:13][CH:14]=2)[CH:9]=1)[CH2:3][CH2:4][C:5](Cl)=[O:6].[Cl-].[Al+3].[Cl-].[Cl-].Cl>ClC(Cl)C(Cl)Cl>[CH3:1][N:2]1[C:8]2[CH:17]=[CH:16][C:15]3[CH:14]=[CH:13][CH:12]=[C:11]([CH2:18][CH2:19][NH:20][C:21](=[O:29])[CH2:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)[C:10]=3[C:9]=2[C:5](=[O:6])[CH2:4][CH2:3]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
The product obtained in Step C (3 mmol), dissolved in 1,1,2,2-tetrachloroethane (30 ml), is added dropwise to a solution of aluminium chloride (10 mmol) in the same solvent (20 ml) under nitrogen. The reaction mixture is heated at 60° C., with stirring, until the reaction has ceased and it is then poured into a mixture of ice (10 g) and concentrated HCl (0.3 ml); stirring is continued for one hour. The aqueous phase is extracted twice with chloroform; the combined organic phases are then dried over magnesium sulphate and concentrated under reduced pressure. The residue is chromatographed on silica gel to yield the title product.
Aufarbeitung
- stirringstirring
- extractionThe aqueous phase is extracted twice with chloroform
- dry with materialthe combined organic phases are then dried over magnesium sulphate
- concentrationconcentrated under reduced pressure
- customThe residue is chromatographed on silica gel
Quellen und Nachweise
- ORD-Eintrag
- ord-cfc3d4e767b840b2b50ad4fd6c6b194c
- Quelldatensatz
- uspto-grants-2006_10
- Patentnummer
- US07115752B2
Verknüpfte Notizen
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