1-Bromo-3-chloropropane → HCID 10934655, Verbindung

HRID 1943101Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1943101
[OH:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:23][CH2:24][CH2:25][Cl:26]>CC(=O)CC>[Cl:26][CH2:25][CH2:24][CH2:23][O:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:14][CH:15]=1

Komponenten

5

Edukt 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 143474-Hydroxybenzophenone

Produkt 1

HCID 10934655HCID 10934655, VerbindungAusbeute 65,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

253.7 g (1.27 mol) 4-hydroxybenzophenone was dissolved in 2.56 l 2-butanone. 884.5 g (6.3 mol) potassium carbonate and 201.5 g (1.27 mol) 1-bromo-3-chloro-propane were added. The mixture was refluxed for 16 hours. The mixture was allowed to cool down to room temperature and the inorganic salts were removed by filtration. The solvent was removed under reduced pressure. The residue was treated with 250 mL acetone and 600 mL isopropyl acetate. The residue partially solidified. The solvent was removed and the residue was treated with 1.5 L water. The crude 4-(3-chloropropoxy)benzophenone crystallized from the medium, was isolated by filtration and dried. 228 g of the crude 4-(3-chloropropoxy)benzophenone was isolated.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 16 hours
  2. customthe inorganic salts were removed by filtration
  3. customThe solvent was removed under reduced pressure
  4. additionThe residue was treated with 250 mL acetone and 600 mL isopropyl acetate
  5. customThe solvent was removed
  6. additionthe residue was treated with 1.5 L water
  7. customThe crude 4-(3-chloropropoxy)benzophenone crystallized from the medium
  8. customwas isolated by filtration
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-78ac8671cf36499bb9f0cefe514c966a
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08389769B2

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