Triethylamine → 5-Methoxy-1-methyl-7-nitro-5-phenyl-1,5-dihydro-2H-1,4-benzodiazepin-2-one

HRID 441487Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 441487
[N+]([N:4]1[C:10]([O:17][CH3:18])([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]2[CH:19]=[C:20]([N+:23]([O-:25])=[O:24])[CH:21]=[CH:22][C:8]=2[N:7]([CH3:26])[C:6](=[O:27])[CH2:5]1)([O-])=O.C(N(CC)CC)C>C(Cl)Cl>[CH3:18][O:17][C:10]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]2[CH:19]=[C:20]([N+:23]([O-:25])=[O:24])[CH:21]=[CH:22][C:8]=2[N:7]([CH3:26])[C:6](=[O:27])[CH:5]=[N:4]1

Komponenten

4

Edukt 2

HCID 8471TriethylamineHCID 12362349HCID 12362349, Verbindung

Produkt 1

HCID 439385-Methoxy-1-methyl-7-nitro-5-phenyl-1,5-dihydro-2H-1,4-benzodiazepin-2-oneAusbeute 56,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 4.7-dinitro-5-methoxy-1-methyl-5-phenyl-1,3,4,5-tetrahydro-2H-1,4-benzodiazepin-2-one (400 mg) and triethylamine (1.1 g) in methylene chloride (10 ml) is allowed to stand at room temperature for 72 hours. The reaction mixture is washed with water, dried over sodium sulfate, and evaporated under reduced pressure to remove the solvent. The residue is washed with diethyl ether to give 5-methoxy-1-methyl-7-nitro-5-phenyl-1,5-dihydro-2H-1,4-benzodiazepin-2-one (196 mg) as crude product.

Aufarbeitung

  1. washThe reaction mixture is washed with water
  2. dry with materialdried over sodium sulfate
  3. customevaporated under reduced pressure
  4. customto remove the solvent
  5. washThe residue is washed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-6e4a5ac633464381b699e0495e1b683e
Quelldatensatz
uspto-grants-1977_08
Patentnummer
US04041026

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