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Azobisisobutyronitrile → HCID 19385590, 화합물

HRID 2255567
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반응식

HRID 2255567 반응식
[CH3:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][CH:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Cl:16])[C:8]#[N:9])=[CH:4][CH:3]=1.C1C(=O)N([Br:26])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:26][CH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Cl:16])[C:8]#[N:9])=[CH:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 193856812-(4-Methylphenoxy)-2-(2'-chlorophenyl)acetonitrile

생성물 1

HCID 19385590HCID 19385590, 화합물수율 72%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To a CCl4 solution (5 mL) of the product (0.200 g) of Step B was added NBS (0.132 g, 0.95 eq) and a catalytic amount of AIBN. The reaction mixture was refluxed overnight. TLC indicated clean conversion to product, and the reaction mixture was cooled to room temperature and concentrated in vacuo. The crude product was purified on a silica gel flash chromatography column (120×30 mm) eluted with 5% ethyl acetate in hexane to afford 0.178 g (72%) of the title compound.

후처리

  1. temperatureThe reaction mixture was refluxed overnight
  2. concentrationconcentrated in vacuo
  3. customThe crude product was purified on a silica gel flash chromatography column (120×30 mm)
  4. washeluted with 5% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-f265e0de1c674ea89dcad06a82438524
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05240938

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