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3-(2-(2,5-Difluorophenyl)hydrazinyl)propanenitrile → HCID 178511141, 화합물

HRID 1466577
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HRID 1466577 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[NH:9][NH:10][CH2:11][CH2:12][C:13]#[N:14]>S(=O)(=O)(O)O.O.S([O-])([O-])(=O)=O.[Fe+3].S([O-])([O-])(=O)=O.S([O-])([O-])(=O)=O.[Fe+3].S([O-])([O-])(=O)=O.[Fe+2]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1/[N:9]=[N:10]/[CH2:11][CH2:12][C:13]#[N:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 668471273-(2-(2,5-Difluorophenyl)hydrazinyl)propanenitrile

생성물 1

HCID 178511141HCID 178511141, 화합물수율 91%

시약·촉매·용매 3

HCID 24393Ferrous Sulfate촉매HCID 167265Ferric sulfate hydrate촉매HCID 1118Sulfuric Acid용매

실험 절차

To a solution of 3-(2-(2,5-difluorophenyl)hydrazinyl)propanenitrile (790 mg) in 15 mL of 2N sulfuric acid was added 2.0 g of iron(III) sulfate hydrate. The reaction mixture was stirred at ambient temperature for 30 min as the iron sulfate slowly dissolved and a yellow oil precipitated. The reaction mixture was extracted with ether, and the extracts were washed with water, brine, dried over sodium sulfate, filtered through a plug of silica gel and concentrated to give 710 mg (91%) of (E)-3-((2,5-difluorophenyl)diazenyl)propanenitrile. LCMS (ESI) m+H=196.2. 1H NMR (400 MHz, CDCl3) δ 7.34-7.08 (m, 3H), 4.54-4.31 (m, 2H), 2.99 (t, 2H).

후처리

  1. dissolutionslowly dissolved
  2. customa yellow oil precipitated
  3. extractionThe reaction mixture was extracted with ether
  4. washthe extracts were washed with water, brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered through a plug of silica gel
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fda8bb9e28b04d598f8243909c36dcef
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999998B2

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