Trifluoroacetic anhydride → HCID 58201206, Verbindung

HRID 882979Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 882979
[Cl:1][C:2]1[C:3]([CH3:12])=[N+:4]([O-])[CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].FC(F)(F)C(OC(=O)C(F)(F)F)=[O:16]>ClCCl.C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([CH2:12][OH:16])=[N:4][CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9]

Komponenten

5

Edukt 2

HCID 9845Trifluoroacetic anhydrideHCID 143691543-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide

Produkt 1

HCID 58201206HCID 58201206, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

The above 3-chloro-4-methoxy-2,5-dimethylpyridine 1-oxide (530 mg) was suspended in 15 ml of dichloromethane, and trifluoroacetic anhydride (0.39 ml) was then added to the suspension under cooling on ice. The resulting mixture was stirred at room temperature for 3 hours. The reaction solution was diluted with chloroform, and was then washed with a saturated sodium bicarbonate solution. The water layer was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (521 mg) as an oily substance.

Aufarbeitung

  1. temperatureunder cooling on ice
  2. washwas then washed with a saturated sodium bicarbonate solution
  3. extractionThe water layer was extracted with chloroform
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. distillationthe solvent was then distilled away

Quellen und Nachweise

ORD-Eintrag
ord-3fd96148a86b4105bd1445093b0714ea
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08236813B2

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