Water → HCID 19068959, Verbindung

HRID 1957218Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1957218
[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-8ab7dda9d82e4969aba388d162b03ace
Quelldatensatz
uspto-grants-1998_07
Patentnummer
US05783575

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