Sodium Hydroxide → HCID 20402696, Verbindung

HRID 1995096Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1995096
[OH-:1].[Na+].Cl.[NH2:4]O.[C:6]([C:14]1[C:15]([NH:21][C:22](=[O:25])[CH2:23]I)=[CH:16][N:17]([CH3:20])[C:18]=1[CH3:19])(=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>O.C(O)C>[C:6]([C:14]1[C:15]([NH:21][C:22](=[O:25])[CH2:23][NH:4][OH:1])=[CH:16][N:17]([CH3:20])[C:18]=1[CH3:19])(=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 20402707HCID 20402707, Verbindung

Produkt 1

HCID 20402696HCID 20402696, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Sodium hydroxide (64 g) was added to a solution of hydroxylamine hydrochloride (111 g) in water (370 ml) and the obtained solution was diluted with ethanol (3500 ml). N-(4-benzoyl-1,5-dimethyl (1H)pyrrol-3-yl)-2-iodoacetamide (124.5 g) was then added and the obtained suspension was stirred under nitrogen stream for about 48 hours. The reaction mixture was filtered in order to remove the salts and the filtrate was concentrated to dryness at the pump. The residue was washed with a small amount of water and crystallized from ethyl acetate yielding 82.5 g of the compound of the title. M.p. 140°-42° C.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered in order
  2. customto remove the salts
  3. concentrationthe filtrate was concentrated to dryness at the pump
  4. washThe residue was washed with a small amount of water
  5. customcrystallized from ethyl acetate yielding 82.5 g of the compound of the title

Quellen und Nachweise

ORD-Eintrag
ord-db163fa095aa45ef80d432858154d889
Quelldatensatz
uspto-grants-1983_09
Patentnummer
US04402970

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