Hydrochloric Acid → 2-(3-Fluoro-4-methylphenyl)benzonitrile

HRID 343956

Reaktionsgleichung

Reaktionsgleichung von HRID 343956
CC1(C)O[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]([F:20])[CH:14]=2)=[N:4]C1.N1C=CC=CC=1.P(Cl)(Cl)(Cl)=O.Cl>CCOCC>[F:20][C:15]1[CH:14]=[C:13]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:5]#[N:4])[CH:18]=[CH:17][C:16]=1[CH3:19]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 24813Phosphorus oxychlorideHCID 545155994,5-Dihydro-5,5-dimethyl-2-(3'-fluoro-4'-methyl-biphenyl-2-yl)oxazole

Produkt 1

HCID 542386242-(3-Fluoro-4-methylphenyl)benzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

97.0 g (343 mmol) of the compound from Example III are initially introduced into 500 ml of pyridine, and 31.3 ml (343 mmol) of phosphorus oxychloride are added at 0° C., while stirring. The mixture is heated slowly, and is finally boiled under reflux for 1 hour. After cooling to room temperature, ether and an amount of 1M hydrochloric acid such that the pH of the aqueous phase is 1.5 are added. The organic phase is washed three more times with 1M sulphuric acid, dried with sodium sulphate and evaporated on a rotary evaporator and the residue is freed from the residual solvent under a high vacuum.

Aufarbeitung

  1. additionare added at 0° C.
  2. temperatureThe mixture is heated slowly
  3. temperatureunder reflux for 1 hour
  4. additionare added
  5. washThe organic phase is washed three more times with 1M sulphuric acid
  6. dry with materialdried with sodium sulphate
  7. customevaporated on a rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-36646c612c374f38a290b8b6f3f05f8f
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05863930

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