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Benzoyl Peroxide → HCID 86617077, 화합물

HRID 706198
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HRID 706198 반응식
[CH2:1]([O:5][C:6]([C:8]1[N:9]=[CH:10][C:11]2[C:16]([C:17]=1[OH:18])=[CH:15][C:14]([S:19]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)(=[O:21])=[O:20])=[CH:13][CH:12]=2)=[O:7])[CH2:2][CH2:3][CH3:4].C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.[Br:46]N1C(=O)CCC1=O>C1C=CC=CC=1>[CH2:1]([O:5][C:6]([C:8]1[N:9]=[C:10]([Br:46])[C:11]2[C:16]([C:17]=1[OH:18])=[CH:15][C:14]([S:19]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)(=[O:21])=[O:20])=[CH:13][CH:12]=2)=[O:7])[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 667135276-Benzenesulfonyl-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester

생성물 1

HCID 86617077HCID 86617077, 화합물수율 75.4%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a mixture of 6-benzenesulfonyl-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester (100 mg, 0.26 mmol; see U.S. Patent Application Publication No. 2004/0254215) and benzene (4.5 mL) was added benzoyl peroxide (6.3 mg, 0.026 mmol). Resulting mixture was refluxed for 15 min. prior to the addition of N-bromosuccinimide (51 mg, 0.29 mmol). Reaction mixture was refluxed overnight. It was concentrated and the crude product was purified by silica gel chromatography (eluting with 20%-80%) ethyl acetate/hexanes to provide the title compound (91 mg). MS-(+)-ion: M+1=466.18, 464.14.

후처리

  1. customResulting mixture
  2. temperaturewas refluxed for 15 min.
  3. customReaction mixture
  4. temperaturewas refluxed overnight
  5. concentrationIt was concentrated
  6. customthe crude product was purified by silica gel chromatography (eluting with 20%-80%) ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-02ab175116384331a588d5128ff4b242
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174976B2

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