1,3-Dibromopropane → 1,3-Bis(2,4-difluoro-6-iodophenoxy)propane

HRID 1468470Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1468470
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([I:9])[C:3]=1[OH:10].Br[CH2:12][CH2:13][CH2:14]Br.[C:16](=[O:19])([O-])[O-].[K+].[K+]>CC(C)=O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([I:9])[C:3]=1[O:10][CH2:12][CH2:13][CH2:14][O:19][C:16]1[C:4]([I:9])=[CH:3][C:2]([F:1])=[CH:7][C:6]=1[F:8]

Komponenten

5

Edukt 3

HCID 80011,3-DibromopropaneHCID 11430Potassium CarbonateHCID 222216242,4-Difluoro-6-iodophenol

Produkt 1

HCID 585165561,3-Bis(2,4-difluoro-6-iodophenoxy)propane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To a solution of 7.68 g (30 mmol) of 2,4-difluoro-6-iodophenol (P7), Preparation 7 and 3.03 g (15 mmol) of 1,3-dibromopropane in 125 mL of acetone add 12.42 g (90 mmol) of potassium carbonate. Reflux the resulting reaction mixture for 48 hours. Cool the reaction mixture to room temperature, filter it, and extract the resulting filtrate thoroughly with methylene chloride. Combine methylene chloride extracts and concentrate them by rotary evaporation. Crystallize the resulting solid from hexanes to yield 3.4 g (41.1%) of (P8) as a white solid.

Aufarbeitung

  1. temperatureReflux
  2. customthe resulting reaction mixture for 48 hours
  3. filtrationfilter it
  4. extractionextract the resulting filtrate thoroughly with methylene chloride
  5. concentrationconcentrate them
  6. customby rotary evaporation
  7. customCrystallize the resulting solid from hexanes
  8. customto yield 3.4 g (41.1%) of (P8) as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-6902d52c34c04724a6c1cfadea210f36
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09000108B2

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