Hydrochloric Acid → HCID 23158218, Verbindung

HRID 601642Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 601642
ClC(Cl)C.[Br:5][C:6]1[C:11]([O:12][CH3:13])=[CH:10][C:9]([O:14][CH3:15])=[CH:8][C:7]=1[F:16].[CH:17]1([CH2:23][C:24](Cl)=[O:25])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.Cl>[Cl-].[Cl-].[Zn+2]>[Br:5][C:6]1[C:7]([F:16])=[C:8]([C:24](=[O:25])[CH2:23][CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[C:9]([O:14][CH3:15])=[CH:10][C:11]=1[O:12][CH3:13]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 63651,1-Dichloroethane3×HCID 6882252-Bromo-3,5-dimethoxy-1-fluorobenzeneHCID 2757989Cyclohexylacetyl chloride

Produkt 1

HCID 23158218HCID 23158218, VerbindungAusbeute 22,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3007855ZincchlorideKatalysator

Versuchsvorschrift

Under nitrogen atmosphere, 6 ml of dichloroethane solution with 2.3 g of 2-bromo-3,5-dimethoxy-1-fluorobenzene and 6 ml of dichloroethane solution with 2.3 g of cyclohexylacetylchloride were dropped sequentially to 15 ml of dichloroethane solution with 1.8 g of alminium trichloride, 180 mg of zinc dichloride at −10° C., and then the mixture was stirred at room temperature for 2 hours. 20% of hydrochloric acid solution was added to the reaction solution, extracted with chloroform. Chloroform layer was washed with saturated saline solution and then dried with anhydrous sodium sulfate. After distilling out the solvents under reduced pressure, residues were separated and purified with silicagel chromatography (hexane/ethyl acetate=5/1) to obtain 780 mg of the above compound as a white solid.

Aufarbeitung

  1. extractionextracted with chloroform
  2. washChloroform layer was washed with saturated saline solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationAfter distilling out the solvents under reduced pressure, residues
  5. customwere separated
  6. custompurified with silicagel chromatography (hexane/ethyl acetate=5/1)

Quellen und Nachweise

ORD-Eintrag
ord-29dd371dbeab4b048706b212ca484592
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07902369B2

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