Methanol → Methyl 4-bromo-2,5-difluorobenzoate

HRID 452461

Reaktionsgleichung

Reaktionsgleichung von HRID 452461
[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:12])[CH:3]=1.[CH3:13]O>>[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([O:8][CH3:13])=[O:7])=[C:4]([F:12])[CH:3]=1

Komponenten

3

Edukt 2

HCID 887MethanolHCID 8228574-Bromo-2,5-difluorobenzoic acid

Produkt 1

HCID 66887346Methyl 4-bromo-2,5-difluorobenzoate

Versuchsvorschrift

4-bromo-2,5-difluorobenzoic acid (4.82 g, 20.3 mmol) and methanol (100 ml, saturated with gaseous HCl) was heated at 65° C. for 3 h. The volatiles were evaporated, MeOH was added and once again it was evaporated. This procedure was repeated three times. Purification by flash column chromatography (isooctane/EtOAc 4:1) gave the title compound (4.2 g). MS m/z (rel. intensity, 70 eV) 252 (M+, 33), 250 (M+, 34), 221 (95), 219 (bp), 193 (20), 191 (21), 112 (32).

Aufarbeitung

  1. customThe volatiles were evaporated
  2. additionMeOH was added
  3. customonce again it was evaporated
  4. customPurification by flash column chromatography (isooctane/EtOAc 4:1)

Quellen und Nachweise

ORD-Eintrag
ord-e7d8122d4d2541f782692e9081313de3
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08492372B2

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