1,3-Dimethyladamantane → 1-Bromo-3,5-dimethyladamantane
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
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
- temperatureSlowly heat
- temperatureunder reflux
- temperatureto cool
- additionpour onto ice water
- extractionThen extract with ether
- washwash the combined organic phases with sodium bicarbonate solution
- dry with materialdry with magnesium sulfate
- filtrationfilter
- customevaporate to dryness under vacuum
- 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
反応ノート
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