1,3-Dimethyl-2-imidazolidinone → 3,4-Difluoro-2-hydroxybenzoic acid

HRID 1276824

Reaktionsgleichung

F[C:2]1[C:10]([F:11])=[C:9]([F:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH-].[Na+].CN1CCN(C)C1=[O:22]>O>[F:11][C:10]1[C:9]([F:12])=[CH:8][CH:7]=[C:3]([C:4]([OH:6])=[O:5])[C:2]=1[OH:22]

Komponenten

Reaktionsbedingungen

Temperatur: 150 °C

Versuchsvorschrift

1.76 g (0.01 mole) of 2,3,4-trifluorobenzoic acid, 1.62 g (0.04 mole) of powdery 99% sodium hydroxide and 20 ml of 1,3-dimethyl-2-imidazolidinone were fed into a 100-ml four-necked flask provided with a thermometer, a stirrer and a reflux condenser. The mixture was stirred at 150° C. for 2 hours to give rise to a reaction. After the completion of the reaction, part of 1,3-dimethyl-2-imidazolidinone was recovered. The resulting reaction mixture was diluted with 500 ml of water and then subjected to precipitation with a 10% aqueous hydrochloric acid solution. The resulting material was cooled in an ice bath. The resulting crystals were collected by filtration, washed with water, and dried to obtain 1.66 g of 3,4-difluorosalicylic acid. The isolated yield was 95.1% relative to the 2,3,4-trifluorobenzoic acid used.

Aufarbeitung

customprovided with a thermometer, a stirrer and a reflux condenser
customto give rise
customto a reaction
customwas recovered
customThe resulting reaction mixture
customsubjected to precipitation with a 10% aqueous hydrochloric acid solution
temperatureThe resulting material was cooled in an ice bath
filtrationThe resulting crystals were collected by filtration
washwashed with water
customdried

Quellen und Nachweise

ORD-Eintrag: ord-210d2c0213b541a2adb95534b5747799
Quelldatensatz: uspto-grants-2000_12
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06166246

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