Pyridine → HCID 73852152, Verbindung

HRID 723229

Reaktionsgleichung

Reaktionsgleichung von HRID 723229
Cl.[NH2:2][OH:3].[Br:4][C:5]1[CH:6]=[C:7]([CH:13]=O)[S:8][C:9]=1[N+:10]([O-:12])=[O:11].N1C=CC=CC=1>CCO>[Br:4][C:5]1[CH:6]=[C:7]([CH:13]=[N:2][OH:3])[S:8][C:9]=1[N+:10]([O-:12])=[O:11]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 218862814-Bromo-5-nitrothiophene-2-carbaldehyde

Produkt 1

HCID 73852152HCID 73852152, VerbindungAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Hydroxylamine hydrochloride (85 g, 1.2 mol) was added to a solution of 4-bromo-5-nitro-thiophene-2-carbaldehyde (234 mg, 0.529 mmol, Example 286: step a) in EtOH (7.5 mL, 200 proof—anhydrous):pyridine (100 mL, anhydrous) at rt over 5 min. The reaction mixture was heated to reflux overnight, then cooled to rt. The solvents were removed in vacuo resulting in a solid residue that was washed with water and filtered. The solid was dried overnight under high vacuum to afford the title compound as a yellow solid (225 g, 88%). The solid was used for the next step without further characterization.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux overnight
  3. customThe solvents were removed in vacuo
  4. customresulting in a solid residue that
  5. washwas washed with water
  6. filtrationfiltered
  7. customThe solid was dried overnight under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-43f2ba13baec47cf9648112fe3674629
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07138530B2

Verknüpfte Notizen

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