Methanol → 5-Bromo-3-fluoro-2-nitroanisole

HRID 914195Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 914195
[Br:1][C:2]1[CH:3]=[C:4](F)[C:5]([N+:9]([O-:11])=[O:10])=[C:6]([F:8])[CH:7]=1.[OH-:13].[K+].[CH3:15]O>>[Br:1][C:2]1[CH:3]=[C:4]([O:13][CH3:15])[C:5]([N+:9]([O-:11])=[O:10])=[C:6]([F:8])[CH:7]=1

Komponenten

4

Edukt 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 213354875-Bromo-1,3-difluoro-2-nitrobenzene

Produkt 1

HCID 579556485-Bromo-3-fluoro-2-nitroanisoleAusbeute 63 %

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

To a solution of 5-bromo-1,3-difluoro-2-nitrobenzene (2.7 g, 11.3 mmol) in methanol (20 mL) was added potassium hydroxide (680 mg, 12 mmol). The reaction mixture was refluxed at 90° C. for 1 h. It was then concentrated, diluted to ethyl acetate and washed by water and brine. The mixture was then purified by flash column to give the product as red oil (1.8 g, 63%). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 3.94 (s, 3H) 7.01 (s, 1H) 7.04 (d, J=8 Hz, 1H).

Aufarbeitung

  1. concentrationIt was then concentrated
  2. additiondiluted to ethyl acetate
  3. washwashed by water and brine
  4. customThe mixture was then purified by flash column

Quellen und Nachweise

ORD-Eintrag
ord-03fa490821344bc78564c9bffc6e4fda
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08026234B2

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