1,3-Dimethyladamantane → 1-Bromo-3,5-dimethyladamantane

HRID 346101

Reaktionsgleichung

Reaktionsgleichung von HRID 346101
[CH3:1][C:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][C:4]([CH3:12])([CH2:5]3)[CH2:3]1)[CH2:9]2.[Br:13]Br.S([O-])([O-])=O.[Na+].[Na+]>>[Br:13][C:6]12[CH2:11][C:2]3([CH3:1])[CH2:9][CH:8]([CH2:10][C:4]([CH3:12])([CH2:3]3)[CH2:5]1)[CH2:7]2

Komponenten

4

Edukt 3

HCID 128001,3-DimethyladamantaneHCID 24408Bromine2×HCID 24437Sodium Sulfite

Produkt 1

HCID 983171-Bromo-3,5-dimethyladamantaneAusbeute 83 %

Versuchsvorschrift

Mix 0.5 mol of 1,3-dimethyl adamantane with a ten times excess of bromine (5 mol). Slowly heat and stir for 4 hrs under reflux. Subsequently, allow to cool and pour onto ice water. Decompose the excess bromine with sodium sulfite until discoloration of the aqueous solution. Then extract with ether, wash the combined organic phases with sodium bicarbonate solution, dry with magnesium sulfate, filter and evaporate to dryness under vacuum. Recrystallize the residue from methanol. (Yield: 83%).

Aufarbeitung

  1. temperatureSlowly heat
  2. temperatureunder reflux
  3. temperatureto cool
  4. additionpour onto ice water
  5. extractionThen extract with ether
  6. washwash the combined organic phases with sodium bicarbonate solution
  7. dry with materialdry with magnesium sulfate
  8. filtrationfilter
  9. customevaporate to dryness under vacuum
  10. customRecrystallize the residue from methanol

Quellen und Nachweise

ORD-Eintrag
ord-22db755042fc49e5815d542cc3bd86e6
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05061703

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