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Water → HCID 22321558, Verbindung

HRID 496551
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 496551
[N+](=[CH:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][N:7]=1)=[O:5])=[N-].FC(F)(F)C(O)=[O:15].O>C(OCC)C>[OH:15][CH2:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][N:7]=1)=[O:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 73882386HCID 73882386, Verbindung

Produkt 1

HCID 22321558HCID 22321558, VerbindungAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

2-Diazo-1-(5-methylisoxazol-3-yl)ethanone (7.0 g, 46 mmol) was dissolved in diethyl ether (100 ml) and trifluoroacetic acid (25 ml) and water (100 ml) were added. The solution was stirred at room temperature for 2 hours, then the diethyl ether was removed in vacuo and the aqueous solution was stirred at room temperature for 18 hours. Further water (100 ml) was added and the aqueous solution was extracted twice with ethyl acetate. The organic extracts were washed successively with water, 10% aqueous potassium carbonate solution and brine, and dried (Na2SO4). Evaporation of the solvent yielded the title-compound as a pale solid (4.0 g, 61%), 1H NMR (360 MHz, CDCl3) 2.52 (3H, s), 4.90 (2H, s), 6.44 (1H, s).

Aufarbeitung

  1. customthe diethyl ether was removed in vacuo
  2. stirringthe aqueous solution was stirred at room temperature for 18 hours
  3. additionFurther water (100 ml) was added
  4. extractionthe aqueous solution was extracted twice with ethyl acetate
  5. washThe organic extracts were washed successively with water, 10% aqueous potassium carbonate solution and brine
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-d342fd922f664990a433ca57590d5266
Quelldatensatz
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06946461B2

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