HCID 178470035, Verbindung → HCID 178516647, Verbindung

HRID 639624

Reaktionsgleichung

Reaktionsgleichung von HRID 639624
C(OC(=O)[C:5]1[C:10]([OH:11])=[CH:9][C:8]([C:12]([F:15])([F:14])[F:13])=[N:7][C:6]=1[OH:16])C>Cl>[F:15][C:12]([F:13])([F:14])[C:8]1[N:7]=[C:6]([OH:16])[CH:5]=[C:10]([OH:11])[CH:9]=1

Komponenten

3

Edukt 1

HCID 178470035HCID 178470035, Verbindung

Produkt 1

HCID 178516647HCID 178516647, VerbindungAusbeute 99,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2,4-Dihydroxy-6-trifluoromethyl-nicotinic acid ethyl ester (62 g/247 mmols) was added in several portions over 30 mins to 6M HCl(aq) (620 mls) at reflux. The resulting mixture was then heated at 100° C. overnight with vigorous stirring to obtain complete solution. The solution was then allowed to cool and concentrated in vacuo to a white solid. This was slurried in water (250 mls) and adjusted to pH 7 with conc. ammonia to get heavy white suspension. The resulting solid was collected by filtration, rinsed through with fresh water, and dried to provide the title compound (44.0 g) as a white solid.

Aufarbeitung

  1. temperatureat reflux
  2. customto obtain complete solution
  3. temperatureto cool
  4. concentrationconcentrated in vacuo to a white solid
  5. customto get heavy white suspension
  6. filtrationThe resulting solid was collected by filtration
  7. washrinsed through with fresh water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f3aba04b1d624006845308eb4c12e6ca
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07691877B2

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