Hydrochloric Acid → 2-Nitro-4-(trifluoromethyl)phenol

HRID 28246

Reaktionsgleichung

Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[Cl-].C(CCCCCCCCCCCC[NH+](C)C)C1C=CC=CC=1.[OH-:38].[K+].Cl>COCCO>[N+:12]([C:3]1[CH:4]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:7][C:2]=1[OH:38])([O-:14])=[O:13]

Komponenten

Reaktionsbedingungen

Temperatur: 65 °C

Versuchsvorschrift

45 g of 4-chloro-3-nitro-benzotrifluoride and 10 ml of 50% strength aqueous benzyldodecyldimethylammonium chloride are initially introduced into 150 ml of ethylene glycol monomethyl ether, and 100 g of 50% strength potassium hydroxide solution are added dropwise in the course of about 30 minutes, up to a temperature of 65° C. The mixture is then stirred at 65° C. for 6 hours and subsequently cooled and rendered acid with concentrated hydrochloric acid, and about 500 ml of distillate are driven over with steam. The organic phase is separated off and washed with 20 ml of dilute hydrochloric acid, and the organic phase is again separated off and dried with sodium sulphate. 38 g of 2-nitro-4-trifluoromethylphenol are obtained, which corresponds to a yield of 92% of theory.

Aufarbeitung

additionare added dropwise in the course of about 30 minutes, up to a temperature of 65° C
temperaturesubsequently cooled
customThe organic phase is separated off
washwashed with 20 ml of dilute hydrochloric acid
customthe organic phase is again separated off
dry with materialdried with sodium sulphate

Quellen und Nachweise

ORD-Eintrag: ord-dd14553770ba48f4a69e66321c63b24e
Quelldatensatz: uspto-grants-1980_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04225731

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