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Benzoyl Peroxide → HCID 57655944, 화합물

HRID 2041332
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HRID 2041332 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH2:10][C:11]([CH3:20])([C:16]([F:19])([F:18])[F:17])[C:12]([F:15])([F:14])[F:13])=[O:9])=[CH:4][CH:3]=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.O>[Br:28][CH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH2:10][C:11]([CH3:20])([C:16]([F:19])([F:17])[F:18])[C:12]([F:13])([F:14])[F:15])=[O:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 57656139HCID 57656139, 화합물

생성물 1

HCID 57655944HCID 57655944, 화합물수율 55%

시약·촉매·용매 2

HCID 962Water용매HCID 5943Carbon Tetrachloride용매

실험 절차

To 1-methyl-4-(3,3,3-trifluoro-2-methyl-2-trifluoromethylpropane-1-sulfinyl)-benzene (4.13 g, 13.0 mmol) in carbon tetrachloride (50 mL) add NBS (2.31 g, 13.0 mmol), benzoyl peroxide (314 mg, 1.30 mmol) and stir overnight at reflux. Cool to ambient temperature, dilute with water and extract three times with EtOAc. Dry over anhydrous Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1) to give the title compound as colorless oil (2.3 g, 55%).

후처리

  1. temperatureat reflux
  2. extractionextract three times with EtOAc
  3. dry with materialDry over anhydrous Na2SO4
  4. concentrationconcentrate in vacuo
  5. customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)

출처 및 근거

ORD 기록
ord-fa9f341384cf463ea06cdab414383daf
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08580780B2

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