Acetic Anhydride → HCID 67348858, Verbindung

HRID 910577Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 910577
[CH2:1]([C:8]1[C:9](=[O:16])[NH:10][NH:11][C:12]=1[CH:13]([CH3:15])[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>O1CCCC1.C(O)(=O)C>[C:17]([N:11]1[C:12]([CH:13]([CH3:14])[CH3:15])=[C:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:9](=[O:16])[NH:10]1)(=[O:19])[CH3:18]

Komponenten

5

Edukt 2

HCID 7918Acetic AnhydrideHCID 673516914-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one

Produkt 1

HCID 67348858HCID 67348858, VerbindungAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

4-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (1.50 g) was dissolved in tetrahydrofuran (6.0 g) at room temperature. Acetic anhydride (0.708 g) and acetic acid (0.0208 g) was added to the solution successively. After the reaction mixture was stirred at room temperature for 15 hours, the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (The product was eluted with dichloromethane at first, and then n-hexane/ethyl acetate=4/1) to give 1-acetyl-4-benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (1.38 g).

Aufarbeitung

  1. customthe solvent was removed under reduced pressure
  2. customThe residue was purified by column chromatography on silica gel (The product
  3. washwas eluted with dichloromethane at first, and then n-hexane/ethyl acetate=4/1)

Quellen und Nachweise

ORD-Eintrag
ord-579bd2bac8bb45139b4b49b6448392db
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08022192B2

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