Methanol → Methyl 3,5-difluoro-4-hydroxybenzoate

HRID 602020Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 602020
C([O:8][C:9]1[C:16]([F:17])=[CH:15][C:12]([C:13]#N)=[CH:11][C:10]=1[F:18])C1C=CC=CC=1.S(=O)(=O)(O)O.[CH3:24][OH:25].[OH2:26]>>[F:18][C:10]1[CH:11]=[C:12]([CH:15]=[C:16]([F:17])[C:9]=1[OH:8])[C:13]([O:25][CH3:24])=[O:26]

Komponenten

5

Edukt 4

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 574457224-Benzyloxy-3,5-difluorobenzonitrile

Produkt 1

HCID 53847253Methyl 3,5-difluoro-4-hydroxybenzoate

Versuchsvorschrift

4-Benzyloxy-3,5-difluorobenzonitrile and 15 ml of concentrated sulfuric acid were added to 100 ml of methanol and the mixture was heated under reflux for 5 days. Then, water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 4.5 g of methyl 3,5-difluoro-4-hydroxybenzoate represented by the formula:

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 days
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2c973720dd154a42bdb4037a1ae8f35c
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07902400B2

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