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Azobisisobutyronitrile → HCID 59557730, 화합물

HRID 425039
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HRID 425039 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([C:8]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)=[O:9])[CH:7]=1.C1C(=O)N([Br:25])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([C:8]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][Br:25])=[CH:12][CH:11]=2)=[O:9])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 23560508HCID 23560508, 화합물

생성물 1

HCID 59557730HCID 59557730, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

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온도
90 °C

실험 절차

To a solution of (5-bromo-2-chlorophenyl)(p-tolyl)methanone (intermediate AG) (16 g, 48.9 mmol) in CCl4 (80 mL), NBS (10.08 g, 57 mmol) and AIBN (0.848 g) was added. Then the mixture was heated to 90° C. After 3 h, CCl4 was removed under reduced pressure. The residue was dissolved in CH2Cl2 and the solution was washed 1× with HCl (1M) and 2× with brine prior to drying over Na2SO4. Solvent was removed under reduced pressure to obtain crude intermediate AH (20.75 g).

후처리

  1. customCCl4 was removed under reduced pressure
  2. dissolutionThe residue was dissolved in CH2Cl2
  3. washthe solution was washed 1× with HCl (1M) and 2× with brine
  4. dry with materialto drying over Na2SO4
  5. customSolvent was removed under reduced pressure
  6. customto obtain crude intermediate AH (20.75 g)

출처 및 근거

ORD 기록
ord-5353343df86c44debcb2a256a4604e10
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106021B2

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