Bromine → HCID 2825186、化合物

HRID 346096ノート

反応式

HRID 346096 の反応式
[CH:1]([C:4]12[CH2:13][CH:8]3[CH2:9][CH:10]([CH2:12][CH:6]([CH2:7]3)[CH2:5]1)[CH2:11]2)([CH3:3])[CH3:2].[Br:14]Br.S([O-])([O-])=O.[Na+].[Na+]>>[Br:14][C:6]12[CH2:12][CH:10]3[CH2:9][CH:8]([CH2:13][C:4]([CH:1]([CH3:3])[CH3:2])([CH2:11]3)[CH2:5]1)[CH2:7]2

参加物

4

反応物 3

HCID 24408Bromine2 回HCID 24437Sodium SulfiteHCID 5244831-isopropyladamantane

生成物 1

HCID 2825186HCID 2825186、化合物収率 83%

実験手順

Mix 0.034 mol of isopropyl adamantane (IV) with a ten times excess of bromine (0.33 mol). Heat slowly and stir under reflux for 4 h. Subsequently, allow to cool and pour onto ice water. Decompose the excess bromine with sodium sulfite until the aqueous solution has discolored. 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. temperatureHeat slowly
  2. temperatureunder reflux for 4 h
  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-e6f21f6a1ffb489a8c560faff0c039a8
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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