Acetic Anhydride → HCID 178474373, Verbindung

HRID 1951430Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1951430
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[C:15]([NH2:16])=[CH:14][NH:13][N:12]=2)=[O:10])=[CH:4][CH:3]=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[C:15]([NH:16][C:17](=[O:19])[CH3:18])=[CH:14][NH:13][N:12]=2)=[O:10])=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 178508056HCID 178508056, Verbindung

Produkt 1

HCID 178474373HCID 178474373, VerbindungAusbeute 46,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

4-Amino-1H-pyrazole-3-carboxylic acid (4-fluorophenyl)-amide (500 mg; 2.27 mmol) was dissolved in 5 ml of pyridine, treated with acetic anhydride (240 μl, 2.5 mmol) then stirred at room temperature overnight. The solvent was removed by evaporation then dichloromethane (20 ml) and 2M hydrochloric acid (20 ml) were added. The undissolved solid was collected by filtration, washed with more dichloromethane and water then dried under vacuum. The product was isolated as an off white solid (275 mg). (LC/MS: Rt 2.96, [M+H]+ 262.91).

Aufarbeitung

  1. customThe solvent was removed by evaporation
  2. additiondichloromethane (20 ml) and 2M hydrochloric acid (20 ml) were added
  3. filtrationThe undissolved solid was collected by filtration
  4. washwashed with more dichloromethane and water
  5. customthen dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-5d46948066ba4db69d89d42a71927eef
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08404718B2

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