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

HRID 572953Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 572953
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([I:9])[CH:3]=1.Br[CH2:11][CH2:12][CH2:13]Br.[C:15](=[O:18])([O-])[O-].[K+].[K+]>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:11][CH2:12][CH2:13][O:18][C:15]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=2[I:9])=[C:4]([I:9])[CH:3]=1

Komponenten

5

Edukt 3

HCID 80011,3-DibromopropaneHCID 11430Potassium CarbonateHCID 101714174-Fluoro-2-iodophenol

Produkt 1

HCID 667805951,3-Bis(4-fluoro-2-iodophenoxy)propane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To a solution of 15.00 g (63.03 mmol) of 4-fluoro-2-iodophenol (P7), Preparation 7 and 6.40 g (31.68 mmol) of 1,3-dibromopropane in 200 mL of acetone add 26.00 g (188.4 mmol) of potassium carbonate. Reflux the resulting reaction mixture for 24 hours. Cool the reaction mixture to room temperature, filter it, and concentrate the filtrate by rotary evaporation. Crystallize the resulting solid from acetonitrile to yield 12.00 g (74%) of (P8) as a white crystalline solid.

Aufarbeitung

  1. temperatureReflux
  2. customthe resulting reaction mixture for 24 hours
  3. filtrationfilter it
  4. concentrationconcentrate the filtrate
  5. customby rotary evaporation
  6. customCrystallize the resulting solid from acetonitrile
  7. customto yield 12.00 g (74%) of (P8) as a white crystalline solid

Quellen und Nachweise

ORD-Eintrag
ord-d97b5df56a5a4d84ba81625083555a2a
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029487B2

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