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

HRID 346101

반응식

HRID 346101 반응식
[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

참가 물질

4

반응물 3

HCID 128001,3-DimethyladamantaneHCID 24408Bromine2회HCID 24437Sodium Sulfite

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-22db755042fc49e5815d542cc3bd86e6
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05061703

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