Sodium Hydroxide → HCID 178517852, Verbindung

HRID 1448417Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1448417
C(OC(=O)C[O:6][C:7]1[C:12]([Cl:13])=[CH:11][C:10]([Cl:14])=[C:9]([F:15])[N:8]=1)C.[OH-].[Na+]>[Ni].O>[F:15][C:9]1[N:8]=[C:7]([OH:6])[C:12]([Cl:13])=[CH:11][C:10]=1[Cl:14]

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 21522711Ethyl [(3,5-dichloro-6-fluoropyridin-2-yl)oxy]acetate

Produkt 1

HCID 178517852HCID 178517852, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

To a 500 milliliter nickel lined reaction bomb was added 10 grams (0.05 mole) of 3,5-dichloro-2,6-difluoropyridine (prepared as above, Example I), 4.4 grams (0.11 mole) of sodium hydroxide and 65 milliliters of water. The bomb was sealed and the reaction carried out at 125° C. for 21/2 hours. At the completion of the reaction, the bomb was opened and the contents, which consisted of a crystalline meterial and a dark liquid, were removed. The mixture was heated until the crystals went into solution. Activated charcoal was added and the mixture filtered through diatomaceous earth. The solution was acidified, cooled and filtered to recover the crude 6-fluoro-3,5-dichloro-2-pyridinol product as a solid. The product was purified by recrystallization from hot benzene and recovered as white crystals melting at 136°-140° C. The product was recovered in a yield of 3.2 grams (31.7 percent). The structure of the product was analyzed by infrared. Upon elemental analysis, the product was found to have carbon, hydrogen, chlorine, fluorine and nitrogen contents of 33.6, 1.3, 37.2, 10.7 and 7.7 percent, respectively, as compared with the theoretical contents of 33.0, 1.1, 38.9, 10.5 and 7.7 percent, respectively, calculated for the above named compound.

Aufarbeitung

  1. customreaction bomb
  2. customThe bomb was sealed
  3. customcarried out at 125° C. for 21
  4. custom2 hours
  5. customAt the completion of the reaction
  6. customa dark liquid, were removed
  7. temperatureThe mixture was heated until the crystals
  8. additionActivated charcoal was added
  9. filtrationthe mixture filtered through diatomaceous earth
  10. temperaturecooled
  11. filtrationfiltered
  12. customto recover the crude 6-fluoro-3,5-dichloro-2-pyridinol product as a solid
  13. customThe product was purified by recrystallization from hot benzene
  14. customrecovered as white crystals melting at 136°-140° C
  15. customThe product was recovered in a yield of 3.2 grams (31.7 percent)

Quellen und Nachweise

ORD-Eintrag
ord-5405cad1e8834a0aaf114ab625a47a6e
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04180395

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