Hydroxylamine → HCID 178513288, Verbindung

HRID 859610Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 859610
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:27]=[CH:26][C:11]3[N:12]=[C:13]([C:18]4[CH:19]=[C:20]([CH:23]=[CH:24][CH:25]=4)[C:21]#[N:22])[CH2:14][C:15](=[O:17])[NH:16][C:10]=3[CH:9]=2)=[CH:4][CH:3]=1.[NH2:28][OH:29]>CCO.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:27]=[CH:26][C:11]3[N:12]=[C:13]([C:18]4[CH:19]=[C:20]([CH:23]=[CH:24][CH:25]=4)[C:21]([NH:28][OH:29])=[NH:22])[CH2:14][C:15](=[O:17])[NH:16][C:10]=3[CH:9]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 2

HCID 787HydroxylamineHCID 97987263-[7-(4-Fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-benzonitrile

Produkt 1

HCID 178513288HCID 178513288, VerbindungAusbeute 86,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred suspension of 3-[7-(4-fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-benzonitrile (Example 57) (355 mg, 1 mmol) in EtOH (60 mL) was added at 23° C. over 6 h 50% aqueous hydroxylamine solution (3.48 mL, 60 mmol) in 6 portions. The mixture was cooled in the ice-bath, diluted with H2O (100 mL) and stirred for 1 h. The precipitate was collected by filtration, washed with water and Et2O, and triturated with ethyl acetate to give the title compound as light yellow solid (336 mg).

Aufarbeitung

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with water and Et2O
  3. customtriturated with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c6821316c05f4d7c86f1695c18a6ec61
Quelldatensatz
uspto-grants-2006_12
Patentnummer
US07151098B2

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