Bromine → 1-Bromo-3-ethyladamantane

HRID 346105

反応式

HRID 346105 の反応式
[CH2:1]([C:3]12[CH2:12][CH:7]3[CH2:8][CH:9]([CH2:11][CH:5]([CH2:6]3)[CH2:4]1)[CH2:10]2)[CH3:2].[Br:13]Br.S([O-])([O-])=O.[Na+].[Na+]>>[Br:13][C:5]12[CH2:11][CH:9]3[CH2:8][CH:7]([CH2:12][C:3]([CH2:1][CH3:2])([CH2:10]3)[CH2:4]1)[CH2:6]2

参加物

4

反応物 3

HCID 24408Bromine2 回HCID 24437Sodium SulfiteHCID 5226371-Ethyladamantane

生成物 1

HCID 27355671-Bromo-3-ethyladamantane収率 83%

実験手順

Mix 0.034 mol of ethyl adamantane with a ten times excess of bromine (0.33 mol). Heat slowly and stir under reflux for 4 hrs. Then allow to cool and pour onto ice water. Decompose the excess bromine with sodium sulfite until discoloration of the aqueous solution. Subsequently 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. temperatureHeat slowly
  2. temperatureunder reflux for 4 hrs
  3. temperatureto cool
  4. additionpour onto ice water
  5. extractionSubsequently 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-615d3b11111c44609f0f8bf0716b3eb3
出典データセット
uspto-grants-1991_10
特許番号
US05061703

関連ノート

読み込み中…