Hydrochloric Acid → HCID 107657770, Verbindung

HRID 629438Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 629438
F[C:2]1[C:10]([F:11])=[C:9]([CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH-].[Na+].CS(C)=[O:17].Cl>O.C(OCC)(=O)C>[F:11][C:10]1[C:2]([OH:17])=[C:3]([CH:7]=[CH:8][C:9]=1[CH3:12])[C:4]([OH:6])=[O:5]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 14798Sodium HydroxideHCID 27741412,3-Difluoro-4-methylbenzoic acid

Produkt 1

HCID 107657770HCID 107657770, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A mixture of 2,3-difluoro-4-methylbenzoic acid (25.0 g), sodium hydroxide (23.2 g) and DMSO (250 mL) was stirred at 140° C. for 12 hr, and then overnight at room temperature, under argon atmosphere. To the reaction mixture was added 6M hydrochloric acid (100 mL) under ice-cooling. Ethyl acetate and water were added thereto at room temperature, the organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (24.3 g). This compound was used in the next step without an additional purification.

Aufarbeitung

  1. customovernight
  2. customat room temperature
  3. temperaturecooling
  4. customat room temperature, the organic layer was separated
  5. extractionthe aqueous layer was extracted with ethyl acetate
  6. washwashed with water and saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6850f4b51435453d999b79af8b94edfb
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09315458B2

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