3,4-Dichlorobenzyl chloride → 4-(4-Chlorobenzoyl)-1-(3,4-dichlorobenzyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on

HRID 2417454Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2417454
[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+].[Cl:24][C:25]1[CH:26]=[C:27]([CH:30]=[CH:31][C:32]=1[Cl:33])[CH2:28]Cl.C(OCC)(=O)C>CN(C=O)C>[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[N:11]([CH2:28][C:27]3[CH:30]=[CH:31][C:32]([Cl:33])=[C:25]([Cl:24])[CH:26]=3)[C:10](=[O:19])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 76093,4-Dichlorobenzyl chlorideHCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 226325544-(4-Chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on

Produkt 1

HCID 226323454-(4-Chlorobenzoyl)-1-(3,4-dichlorobenzyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

20 mg (0.067 mmol) of 4-(4-chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on was dissolved in 5 ml of DMF. 3 mg (0.08 mmol) of sodium hydride was added to the obtained solution, and they were stirred at room temperature for 30 minutes. 16 mg (0.08 mmol) of 3,4-dichlorobenzyl chloride was added to the obtained mixture and they were stirred at 60° C. overnight. The reaction mixture was treated with ethyl acetate as the extracting solvent by an ordinary method to obtain the crude product. After the purification by the silica gel column chromatography, the title compound was obtained.

Aufarbeitung

  1. stirringwere stirred at 60° C. overnight
  2. customto obtain the crude product
  3. customAfter the purification by the silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-15819476d3dd411d95ae361957dad92d
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06825191B2

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