Water → HCID 19068959, Verbindung

HRID 1735114Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1735114
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2[CH:11]=[CH:12][S:13][C:3]1=2.[F:14][C:15]([F:26])([F:25])[C:16](OC1C=CC=CN=1)=[O:17].[Al+3].[Cl-].[Cl-].[Cl-].O>ClCCCl>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2[C:11]([C:16](=[O:17])[C:15]([F:26])([F:25])[F:14])=[CH:12][S:13][C:3]1=2

Komponenten

6

Edukt 4

HCID 962WaterHCID 46382142-(Trifluoroacetoxy)pyridineHCID 6451240Aluminum(III) ChlorideHCID 19068992HCID 19068992, Verbindung

Produkt 1

HCID 19068959HCID 19068959, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

A mixture of 1 g of (73) and 1.1 g of 2-trifluoromethylcarbonyloxypyridine, prepared according to the literature (Keumi, T. et. al. Chem. Lett. 5 (1990) 783-6), in 25 ml of 1,2-dichloroethane, was cooled to -10° C. with stirring. 1.5 g of AlCl3 was added over 15 minutes at this temperature, the reaction mixture was stirred at 0° C. for 4 hours, and at room temperature overnight. Water was added, the phases separated, and the organic phase dried and evaporated to dryness. Purification by column chromatography on silica gel in toluene gave the pure (74). Yield 590 mg. M.p. 138°-40° C.

Aufarbeitung

  1. customprepared
  2. stirringthe reaction mixture was stirred at 0° C. for 4 hours
  3. customat room temperature
  4. customovernight
  5. customthe phases separated
  6. customthe organic phase dried
  7. customevaporated to dryness
  8. customPurification by column chromatography on silica gel in toluene

Quellen und Nachweise

ORD-Eintrag
ord-0a2765c1086248439f7cef9063d18399
Quelldatensatz
uspto-grants-1996_07
Patentnummer
US05536721

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