Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Cl:11])[CH:10]=1)[C:5](Cl)=[O:6].[NH2:12][N:13]1[CH2:19][CH:18]([O:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:17]2[CH:27]=[C:28]([O:33][CH3:34])[C:29]([O:31][CH3:32])=[CH:30][C:16]=2[CH2:15][CH2:14]1.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Cl:11])[CH:10]=1)[C:5]([NH:12][N:13]1[CH2:19][CH:18]([O:20][C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:17]2[CH:27]=[C:28]([O:33][CH3:34])[C:29]([O:31][CH3:32])=[CH:30][C:16]=2[CH2:15][CH2:14]1)=[O:6]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3,5-Dichlorobenzoyl chloride (1.7 g) was added to a solution of 3-amino-7,8-dimethoxy-1-phenoxy-2,3,4,5-tetrahydro-3-benzazepine (2.1 g) in 100 ml dichloromethane containing sodium bicarbonate (3 g). After one hour, the mixture was filtered and concentrated. The solid residue was eluted through silica with 10% ethyl acetate in dichloromethane to yield 2.4 g of light tan solid, mp 182°-184°. This solid was recrystallized from acetonitrile to yield 2 g of white crystals, mp 184°-185°.
Aufarbeitung
- filtrationthe mixture was filtered
- concentrationconcentrated
- washThe solid residue was eluted through silica with 10% ethyl acetate in dichloromethane
- customto yield 2.4 g of light tan solid, mp 182°-184°
- customThis solid was recrystallized from acetonitrile
Quellen und Nachweise
- ORD-Eintrag
- ord-5113fc8db5c4427cb477426f39177d1a
- Quelldatensatz
- uspto-grants-1993_04
- Patentnummer
- US05202319
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