Carbon Dioxide → 5-Trifluoromethoxysalicylic acid

HRID 1031885

Reaktionsgleichung

Reaktionsgleichung von HRID 1031885
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.[C:13](=O)([O-:15])[O-:14].[K+].[K+].C(=O)=O>O>[OH:10][C:7]1[CH:6]=[CH:5][C:4]([O:3][C:2]([F:11])([F:12])[F:1])=[CH:9][C:8]=1[C:13]([OH:15])=[O:14]

Komponenten

5

Edukt 3

HCID 280Carbon DioxideHCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenol

Produkt 1

HCID 27751035-Trifluoromethoxysalicylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
200 °C

Versuchsvorschrift

178 g (1 mol) of 4-trifluoromethoxyphenol and 345 g (2.5 mol) of potassium carbonate were initially introduced into an autoclave which was then pressurized to 60 bar with carbon dioxide and heated at 200° C. for 4 hours. After cooling and releasing the pressure, the residue was dissolved in 1.5 l of hot water, the solution was filtered hot, the cooled filtrate was extracted using methylene chloride and the extract was clarified using active carbon. The pH was then adjusted to 1 and the precipitated product was filtered off with suction. 192 g of product having a melting point of 129° C. were obtained, which corresponds to 86% of theory.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe solution was filtered hot
  3. extractionthe cooled filtrate was extracted
  4. filtrationthe precipitated product was filtered off with suction
  5. customwere obtained

Quellen und Nachweise

ORD-Eintrag
ord-753b479947974eae883af69265b3ba90
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04956370

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