Ammonia → HCID 178516647, Verbindung

HRID 639706Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 639706
C(OC(=O)[C:5]1[C:10]([OH:11])=[CH:9][C:8]([OH:12])=[N:7][C:6]=1[C:13]([F:16])([F:15])[F:14])C.N>Cl>[F:16][C:13]([F:14])([F:15])[C:6]1[N:7]=[C:8]([OH:12])[CH:9]=[C:10]([OH:11])[CH:5]=1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 178470040HCID 178470040, Verbindung

Produkt 1

HCID 178516647HCID 178516647, VerbindungAusbeute 84,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
115 °C

Versuchsvorschrift

4,6-dihydroxy-2-trifluoromethyl-nicotinic acid ethyl ester (15 g, 59.7 mmol) was dissolved in 250 mL of concentrated HCl and the mixture was stirred at 115° C. for 3 days. The mixture was cooled down to 0° C. and 0.88 ammonia was added until pH˜7. The solid formed was filtered, washed with water, azeotroped with toluene and dried in vacuo to give 9 g of the title compound as a white solid.

Aufarbeitung

  1. temperatureThe mixture was cooled down to 0° C.
  2. customThe solid formed
  3. filtrationwas filtered
  4. washwashed with water
  5. customazeotroped with toluene
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7ba298051d204cfe93f7d545d1b5bb39
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07691877B2

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