Hydrochloric Acid → 2,3-Dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone

HRID 568691

Reaktionsgleichung

Reaktionsgleichung von HRID 568691
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[C:4]([F:11])[CH:3]=1.[Cl:12][C:13]1[C:18]([Cl:19])=[CH:17][CH:16]=[CH:15][C:14]=1[O:20][CH3:21].[Al+3].[Cl-].[Cl-].[Cl-].Cl>ClCCCl>[Cl:19][C:18]1[C:13]([Cl:12])=[C:14]([O:20][CH3:21])[CH:15]=[CH:16][C:17]=1[C:6]([C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][C:4]=1[F:11])=[O:7]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 161262,3-DichloroanisoleHCID 27736014-Chloro-2-fluorobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 140972672,3-Dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

To a mixture of 46 g of 4-chloro-2-fluorobenzoyl chloride and 38.9 g of 2,3-dichloroanisole in 150 ml of 1,2-dichloroethane, 32 g of AlCl3 is added gradually. The mixture is warmed to 40° C. with a vigorous evolution of gas. The mixture is poured into concentrated HCl and ice. The organic layer is separated and the aqueous layer is extracted with additional organic solvent. The combined organic extracts are washed with water, dried over Na2SO4 and evaporated. The crude product is triturated with hexane to give 2,3-dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone. An analytical sample is recrystallized from EtOH, mp 115°-116° C.

Aufarbeitung

  1. additionis added gradually
  2. customThe organic layer is separated
  3. extractionthe aqueous layer is extracted with additional organic solvent
  4. washThe combined organic extracts are washed with water
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. customThe crude product is triturated with hexane

Quellen und Nachweise

ORD-Eintrag
ord-bc590864a6fc47a98ea3d7f652422ddd
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04728662

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