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Ethanol → HCID 19821136, Verbindung

HRID 1029995
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1029995
[OH-].[Na+].C([O:6][C:7]1[CH:12]=[C:11]([NH:13][C:14](=[O:16])[CH3:15])[C:10]([O:17][CH3:18])=[CH:9][C:8]=1[CH3:19])(=O)C.C(O)C>C(O)(=O)C>[CH3:19][C:8]1[CH:9]=[C:10]([O:17][CH3:18])[C:11]([NH:13][C:14](=[O:16])[CH3:15])=[CH:12][C:7]=1[OH:6]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 19821145HCID 19821145, Verbindung

Produkt 1

HCID 19821136HCID 19821136, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

To 35 ml of a 0.4N aqueous solution of sodium hydroxide were added 1.70 g (7.17 mmol) of 2-methyl-4-methoxy-5-acetylaminophenyl acetate and 10 ml of ethanol. The mixture was stirred at room temperature for 10 minutes. When crystals were completely dissolved, the stirring was ceased. Then 0.3 ml of acetic acid was added and thus crystals were precipitated. The crystals were collected by filtration, purified by column chromatography (Silica Gel 60, trade name, manufactured by Merck Co., 230-400 mesh, 200 g, eluent: ethyl acetate) and recrystallized from the solvent mixture of ethyl acetate/hexane (2:1). Thus 1.05 g (5.38 mmol) of 2-methyl-4-methoxy-5-acetylaminophenol was obtained. The yield was 75%.

Aufarbeitung

  1. dissolutionWhen crystals were completely dissolved
  2. customthus crystals were precipitated
  3. filtrationThe crystals were collected by filtration
  4. custompurified by column chromatography (Silica Gel 60, trade name, manufactured by Merck Co., 230-400 mesh, 200 g, eluent: ethyl acetate)
  5. customrecrystallized from the solvent mixture of ethyl acetate/hexane (2:1)

Quellen und Nachweise

ORD-Eintrag
ord-cce48bc9446443a29a1337f064ab5680
Quelldatensatz
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05104414

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