反応 #433283

反応方程式

sodium sulfite

1,3-dimethyl adamantane

bromine

bromine

→

1-Bromo-3,5-dimethyl Adamantane

収率 83.0%

反応条件

後処理

1. 1
   温度Slowly heat
2. 2
   温度under reflux
3. 3
   温度to cool
4. 4
   workup.ADDITIONpour onto ice water
5. 5
   抽出Then extract with ether
6. 6
   洗浄wash the combined organic phases with sodium bicarbonate solution
7. 7
   乾燥dry with magnesium sulfate
8. 8
   ろ過filter
9. 9
   その他evaporate to dryness under vacuum
10. 10
    その他Recrystallize the residue from methanol

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%).

出典