Azobisisobutyronitrile → HCID 86726615, 화합물

HRID 1506148노트

반응식

HRID 1506148 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:10]([F:13])([F:12])[F:11])=[C:6]([CH:9]=1)[C:7]#[N:8].[Br:14]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>ClCCCl>[Br:14][CH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:10]([F:11])([F:12])[F:13])=[C:6]([CH:9]=1)[C:7]#[N:8]

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 177507255-Methyl-2-(trifluoromethyl)benzonitrile

생성물 1

HCID 86726615HCID 86726615, 화합물수율 49.1%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

5-Methyl-2-(trifluoromethyl)benzonitrile (200 mg, 1.08 mmol) in 1,2-dichloroethane (3 mL) was stirred with N-bromosuccinimide (192 mg, 1.08 mmol) and azobisisobutyronitrile (36.1 mg, 0.22 mmol) at 80° C. for 2 hours. The reaction mixture allowed to cool to room temperature and was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane→ethyl acetate/hexane=1/3 (v/v)) to give the title compound as a colorless solid (140 mg, yield 49%).

후처리

  1. concentrationwas concentrated under reduced pressure
  2. customThe residue was purified by silica gel column chromatography (hexane→ethyl acetate/hexane=1/3 (v/v))

출처 및 근거

ORD 기록
ord-1f915a0d7c904efa9360c440c07c214d
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216999B2

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