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Bromine → HCID 69316420, 화합물

HRID 2115154
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HRID 2115154 반응식
[CH2:1]([CH:4]1[CH2:9][CH2:8][CH:7]([CH:10]2[CH2:15][CH2:14][CH:13]([C:16]3[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[Br:23]Br>C(Cl)Cl.ClC1C=CC=CC=1>[Br:23][C:18]1[CH:17]=[C:16]([CH:13]2[CH2:14][CH2:15][CH:10]([CH:7]3[CH2:6][CH2:5][CH:4]([CH2:1][CH2:2][CH3:3])[CH2:9][CH2:8]3)[CH2:11][CH2:12]2)[CH:21]=[CH:20][C:19]=1[OH:22]
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참가 물질

5

반응물 2

HCID 24408BromineHCID 3107829Phenol, 4-(4'-propyl[1,1'-bicyclohexyl]-4-yl)-

생성물 1

HCID 69316420HCID 69316420, 화합물수율 39.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 7964Chlorobenzene용매

실험 절차

4-(4-(4-Propylcyclohexyl)cyclohexyl)phenol (0.5 g) was dissolved in a mixed solvent of methylene chloride (5 ml) and chlorobenzene (1 ml), to which was then added dropwise a solution of bromine (0.28 g) in methylene chloride (2 ml) under ice cooling while stirring. After completion of the dropwise addition, the reaction mixture was stirred at room temperature for 30 minutes, added in ice water, and then extracted with methylene chloride. An organic layer was washed with water, rinsed with a sodium thiosulfate aqueous solution, and then dried over anhydrous magnesium sulfate. The methylene chloride solution was concentrated in vacuo and then subjected to isolation and purification by silica gel column chromatography, thereby obtaining a white crystal (0.25 g) of 2-bromo-4-(4-(4-propylcyclohexyl)cyclohexyl)phenol.

후처리

  1. additionAfter completion of the dropwise addition
  2. stirringthe reaction mixture was stirred at room temperature for 30 minutes
  3. extractionextracted with methylene chloride
  4. washAn organic layer was washed with water
  5. washrinsed with a sodium thiosulfate aqueous solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationThe methylene chloride solution was concentrated in vacuo
  8. customsubjected to isolation and purification by silica gel column chromatography

출처 및 근거

ORD 기록
ord-b94c86d56e814276b1f8b237f4271a31
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07435455B2

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