Bromine → HCID 2825186, 화합물

HRID 346096노트

반응식

HRID 346096 반응식
[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

참가 물질

4

반응물 3

HCID 24408Bromine2회HCID 24437Sodium SulfiteHCID 5244831-isopropyladamantane

생성물 1

HCID 2825186HCID 2825186, 화합물수율 83%

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-e6f21f6a1ffb489a8c560faff0c039a8
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05061703

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