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Azobisisobutyronitrile → HCID 23365403, 화합물

HRID 1080725
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인쇄 미리보기

반응식

HRID 1080725 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:14]2[S:15][CH:16]=[CH:17][CH:18]=2)=[CH:4][CH:3]=1.CC(N=NC(C#N)(C)C)(C#N)C.[Br:31]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:31][CH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:14]2[S:15][CH:16]=[CH:17][CH:18]=2)=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 23365443HCID 23365443, 화합물

생성물 1

HCID 23365403HCID 23365403, 화합물수율 97.5%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A solution of 123 mg (0.492 mmol) of 4-methyl-2'-(2-thienyl)-1,1'-biphenyl, 18.5 mg of AIBN and 110 mg (0.62 mmol) of N-bromosuccinimide in 50 mL of carbon tetrachloride was heated at reflux until a negative starch iodide reaction was obtained (2 hr). The reaction mixture was evaporated under vacuum and the residue triturated with hexane. The hexane washes were filtered and the filtrate evaporated under vacuum to give 158 mg of product. 1H NMR (300 MHz, CDCl3): 4.48 (s, 2H), 6.68 (dd, 1H), 6.88 (dd, 1H), 7.11 (m, 5H), 7.36 (m, 3H), 7.50 (dd, 1H).

후처리

  1. customwas obtained (2 hr)
  2. customThe reaction mixture was evaporated under vacuum
  3. customthe residue triturated with hexane
  4. filtrationThe hexane washes were filtered
  5. customthe filtrate evaporated under vacuum

출처 및 근거

ORD 기록
ord-fdd528b965cc470a956b4af8d34ec523
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05583130

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