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

HRID 346101

反応式

HRID 346101 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 983171-Bromo-3,5-dimethyladamantane収率 83%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-22db755042fc49e5815d542cc3bd86e6
出典データセット
uspto-grants-1991_10
特許番号
US05061703

関連ノート

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