Benzoyl Peroxide → HCID 59610060, 화합물

HRID 1889165노트

반응식

HRID 1889165 반응식
[CH3:1][O:2][C:3](=[O:20])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([CH:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)(=[O:13])=[O:12])=[CH:7][CH:6]=1.C1C(=O)N([Br:28])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl.C(Cl)Cl>[CH3:1][O:2][C:3](=[O:20])[CH:4]([Br:28])[C:5]1[CH:10]=[CH:9][C:8]([S:11]([CH:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)(=[O:12])=[O:13])=[CH:7][CH:6]=1

참가 물질

6

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 59610035HCID 59610035, 화합물

생성물 1

HCID 59610060HCID 59610060, 화합물수율 37.1%

시약·촉매·용매 2

HCID 5943Carbon Tetrachloride용매HCID 6344Dichloromethane용매

실험 절차

[4-(Tetrahydro-pyran-4-sulfonyl)-phenyl]-acetic acid methyl ester (1.60 gm, 5.36 mmol), NBS (1.04 g, 5.90 mmol) and benzoyl peroxide (0.130 g, 0.53 mmol) in carbon tetrachloride (50 ml) was refluxed for 7 hrs. Reaction mixture was diluted with DCM (50 ml), washed with water and brine (100 ml each), dried over anhydrous sodium sulfate, fliltered and concentrated. Crude compound was purified by column chromatography over silica gel using 30% ethyl acetate hexane as eluent to give the pure bromo-[4-(tetrahydro-pyran-4-sulfonyl)-phenyl]-acetic acid methyl ester (0.75 gm).

후처리

  1. customReaction mixture
  2. washwashed with water and brine (100 ml each)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customCrude compound was purified by column chromatography over silica gel using 30% ethyl acetate hexane as eluent

출처 및 근거

ORD 기록
ord-3858e3980014430daaaf6fc249519bec
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501955B2

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