Sodium Hydroxide → 1-(4-Carboxybenzyl)-4-(4-chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on
Reaktionsgleichung
[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[NH:11][C:10](=[O:19])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.[H-].[Na+].Br[CH2:25][C:26]1[CH:35]=[CH:34][C:29]([C:30]([O:32]C)=[O:31])=[CH:28][CH:27]=1.[OH-].[Na+]>CN(C=O)C.C(OCC)(=O)C.C(O)C.C1COCC1>[C:30]([C:29]1[CH:34]=[CH:35][C:26]([CH2:25][N:11]2[C:12]3[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=3[CH2:14][N:8]([C:6](=[O:7])[C:5]3[CH:20]=[CH:21][C:2]([Cl:1])=[CH:3][CH:4]=3)[CH2:9][C:10]2=[O:19])=[CH:27][CH:28]=1)([OH:32])=[O:31]Komponenten
9
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 4
Versuchsvorschrift
300 mg (1.0 mmol) of 4-(4-chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on was dissolved in 10 ml of DMF. 48 mg (1.2 mmol) of sodium hydride was added to the obtained solution, and they were stirred at room temperature for 30 minutes. 300 mg (1.3 mmol) of methyl 4-bromomethylbenzoate was added to the obtained mixture, and they were stirred at 60° C. overnight. After the treatment with ethyl acetate as the extracting solvent, the obtained crude product was stirred together with 2 ml of THF, 2 ml of ethanol and 2 ml of 1 N aqueous sodium hydroxide solution at room temperature overnight. The obtained product was treated with ethyl acetate as the extracting solvent by an ordinary method to obtain the crude product.
Aufarbeitung
- stirringwere stirred at 60° C. overnight
Quellen und Nachweise
- ORD-Eintrag
- ord-205b1ef72a194d9693dacd493e87f40b
- Quelldatensatz
- uspto-grants-2004_11
- Patentnummer
- US06825191B2
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