HCID 21249960, Verbindung → HCID 21249961, Verbindung

HRID 1531657Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1531657
[Br:1][C:2]1[C:3]([O:23][CH3:24])=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][NH:9][CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1>C(OC(=O)CC)(=O)CC.O>[Br:1][C:2]1[C:3]([O:23][CH3:24])=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][N:9]([C:3](=[O:23])[CH2:2][CH3:22])[C:8]([CH3:21])=[CH:7][C:6]=2[CH:22]=1

Komponenten

4

Edukt 1

HCID 21249960HCID 21249960, Verbindung

Produkt 1

HCID 21249961HCID 21249961, VerbindungAusbeute 140,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 31263Propionic anhydrideLösungsmittel

Versuchsvorschrift

0.67 g (1.7 mmol) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine (Example 4, Step A) is suspended in 3.35 ml of propionic acid anhydride and stirred for 3 hours at room temperature. The mixture is diluted with water, and the product is filtered. After washing with water and drying by column chromatography, the crude product is purified (silica gel, eluant benzene:ethyl acetate: 4:0.2). 0.53 g (70%) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-3-propionyl-3H-2,3-benzodiazepine is obtained as a thick oil.

Aufarbeitung

  1. filtrationthe product is filtered
  2. washAfter washing with water
  3. customdrying by column chromatography
  4. customthe crude product is purified (silica gel, eluant benzene:ethyl acetate: 4:0.2)

Quellen und Nachweise

ORD-Eintrag
ord-157306b38e0f425792fb4a2f8c5c3672
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06200970B1

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