HCID 66701185, Verbindung → 4-Fluoro-1-hydroxy-2-naphthoic acid

HRID 1889293Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1889293
[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12]C)=[C:4]([C:14]([OH:16])=[O:15])[CH:3]=1>CC(O)=O>[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([OH:12])=[C:4]([C:14]([OH:16])=[O:15])[CH:3]=1

Komponenten

3

Edukt 1

HCID 66701185HCID 66701185, Verbindung

Produkt 1

HCID 231327944-Fluoro-1-hydroxy-2-naphthoic acidAusbeute 81,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To 10.1 g 4-fluoro-1-methoxynaphthalene-2-carboxylic acid 55 ml HBr/HOAc were added and the mixture was stirred and heated. After 30 min at 60° C. another 7.5 ml of hBr/HOAc were added, and after an additional 30 min at 80° C. the mixture was cooled to ambient temperature and left standing overnight. The reaction was then poured into ice/water and the precipitated solid was filtered and washed with water, followed by 1% ether in heptane and then by heptane. The solid was dried in vacuo at 40° C. to yield 7.7 g 4-fluoro-1-hydroxynaphthalene-2-carboxylic acid.

Aufarbeitung

  1. temperatureheated
  2. waitleft
  3. filtrationthe precipitated solid was filtered
  4. washwashed with water
  5. customThe solid was dried in vacuo at 40° C.

Quellen und Nachweise

ORD-Eintrag
ord-92267d91c9234ed2888c56fa25f7b486
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08501981B2

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