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9-Methylphenanthrene → Phenanthrene, 9-(bromomethyl)-

HRID 868766
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인쇄 미리보기

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HRID 868766 반응식
[CH3:1][C:2]1[C:3]2[C:8]([C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=3[CH:15]=1)=[CH:7][CH:6]=[CH:5][CH:4]=2.C1C(=O)N([Br:23])C(=O)C1>C1C=CC=CC=1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:23][CH2:1][C:2]1[C:3]2[C:8]([C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=3[CH:15]=1)=[CH:7][CH:6]=[CH:5][CH:4]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 134389-MethylphenanthreneHCID 67184N-bromobutanimide

생성물 1

HCID 185571Phenanthrene, 9-(bromomethyl)-수율 89.7%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 241Benzene용매

반응 조건

온도
0 °C

실험 절차

A mixture of 9-methylphenanthrene (14.2 g, 74 mmol), benzoyl peroxide (40 mg, 0.16 mmol) and NBS (13.3 g, 74.6 mmol) in 210 mL of benzene was refluxed for 5 h. The reaction mixture was cooled to 0° C. and the succinimide precipitated was removed by filtration. The filtrate was washed by 15% NaOH, dried over MgSO4 and concentrated to yield 18 g of product which was used for the next step without further purification.

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후처리

  1. temperaturewas refluxed for 5 h
  2. customthe succinimide precipitated
  3. customwas removed by filtration
  4. washThe filtrate was washed by 15% NaOH
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-089e894bbbd949f7a193802e14b14d78
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08968887B2

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