Methanol → HCID 67509641, Verbindung

HRID 623449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 623449
[Cl:1][C:2]1[C:3]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].S(=O)(=O)(O)O.[CH3:22]O>>[Cl:1][C:2]1[C:3]([O:11][CH2:12][C:13]([F:15])([F:16])[F:14])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([O:9][CH3:22])=[O:8]

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 167824855-Chloro-6-(2,2,2-trifluoroethoxy)pyridine-3-carboxylic acid

Produkt 1

HCID 67509641HCID 67509641, VerbindungAusbeute 56 %

Versuchsvorschrift

A mixture of 5-chloro-6-(2,2,2-trifluoroethoxy)nicotinic acid (5.6 g, 21.9 mmol, Step-1 of Amine-5) and sulfuric acid (0.12 mL, 2.25 mmol) in methanol (40 mL) is refluxed with stirring for 2 days. After removal of the solvent, the residue is poured into 2M sodium hydroxide (100 mL) and extracted with ethyl acetate and dried over sodium sulfate and concentrated in vacuo to give 3.28 g (56% yield) of the title compound as a white solid.

Aufarbeitung

  1. temperatureis refluxed
  2. customAfter removal of the solvent
  3. additionthe residue is poured into 2M sodium hydroxide (100 mL)
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-de33234e42ce4e25a6fa438ffcd03b7b
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09302991B2

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