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Bromine → HCID 178432818, Verbindung

HRID 1931218
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1931218
[OH:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=[C:4]([CH3:11])[CH:3]=1.[Br:12]Br>C(O)(=O)C.O>[Br:12][C:3]1[C:4]([CH3:11])=[N:5][CH:6]=[C:7]([C:2]=1[OH:1])[C:8]([OH:10])=[O:9]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 24408BromineHCID 178429106HCID 178429106, Verbindung

Produkt 1

HCID 178432818HCID 178432818, VerbindungAusbeute 98,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

4-Hydroxy-6-methylnicotinic acid 19 (95.6 g, 0.625 mol) was dissolved in acetic acid (950 ml) and water (190 ml), and bromine (39 ml, 0.750 mol) was added over 15 minutes. After the solution was stirred at 60° C. for 5 hours, the solvent was distilled off under reduced pressure, methanol (200 ml) was added and, crystals were collected by filtration. The solution was distilled off under reduced pressure, methanol was added again to the residue, and crystals were collected by filtration. A total of 142.2 g (98%) of 5-bromo-4-hydroxy-6-methylnicotinic acid 20 was obtained as a colorless crystal.

Aufarbeitung

  1. distillationthe solvent was distilled off under reduced pressure, methanol (200 ml)
  2. additionwas added
  3. filtrationcrystals were collected by filtration
  4. distillationThe solution was distilled off under reduced pressure, methanol
  5. additionwas added again to the residue, and crystals
  6. filtrationwere collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-f43285c516d9484a95a3691547922a55
Quelldatensatz
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08188271B2

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