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Benzoyl Peroxide → HCID 22648203, 화합물

HRID 394141
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HRID 394141 반응식
[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])[C:3]=1[CH3:16].[Br:17]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])[C:3]=1[CH2:16][Br:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 226481954,6-Dibromo-2-(2-chlorophenyl)-3-methylpyridine

생성물 1

HCID 22648203HCID 22648203, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To a suspension of 6.3 g of 4,6-dibromo-2-(2-chlorophenyl)-3-methylpyridine (COMPOUND W-1) in 75 mL of CCl4 was added 3.7 g of N-bromosuccinimide and 420 mg of benzoyl peroxide. The mixture was heated to reflux and stirred at this temperature for 6 h, then cooled and concentrated. The residue was dissolved in 150 mL of 1:1 hexanes-Et2O and filtered through a pad of silica gel, then purified in two batches by flash chromatography on Biotage 40M columns, eluting with a gradient system of 99:1 to 97:3 hexanes-Et2O, to yield the title compound as a white solid.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperaturecooled
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in 150 mL of 1:1 hexanes-Et2O
  6. filtrationfiltered through a pad of silica gel
  7. custompurified in two batches by flash chromatography on Biotage 40M columns
  8. washeluting with a gradient system of 99:1 to 97:3 hexanes-Et2O

출처 및 근거

ORD 기록
ord-258a4e1b82c84b9380e48bdac39f1574
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06809199B2

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