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3-(Heptafluoropropyl)-5-methyl-4-nitro-1H-pyrazole → 3-Heptafluoropropyl-5-methyl-1H-pyrazol-4-ylamine

HRID 1372020
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HRID 1372020 반응식
[F:1][C:2]([F:19])([C:15]([F:18])([F:17])[F:16])[C:3]([F:14])([F:13])[C:4]1[C:8]([N+:9]([O-])=O)=[C:7]([CH3:12])[NH:6][N:5]=1>C(O)(=O)C.[Zn]>[F:19][C:2]([F:1])([C:15]([F:17])([F:18])[F:16])[C:3]([F:13])([F:14])[C:4]1[C:8]([NH2:9])=[C:7]([CH3:12])[NH:6][N:5]=1
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참가 물질

4

반응물 1

HCID 27749443-(Heptafluoropropyl)-5-methyl-4-nitro-1H-pyrazole

생성물 1

HCID 210711353-Heptafluoropropyl-5-methyl-1H-pyrazol-4-ylamine

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매2회

실험 절차

To a suspension of zinc dust (1.5 g) in glacial acetic acid (10 mL) was added drop-wise, a solution of 3-Heptafluoropropyl-5-methyl-4-nitro-1H-pyrazole (0.295 g, 1.0 mmol) in glacial acetic acid (5 mL). The reaction mixture was then allowed to stir at room temperature for 14 h. The zinc salts were then removed by filtration and the residue washed with ethyl acetate. The combined organic extract was concentrated in vaccum, re-dissolved in CHCl3, washed with NaHCO3, water and brine. Finally the organic layer was dried with Na2SO4 and solvent evaporated to give the title compound as white solid.

후처리

  1. additionwas added drop-wise
  2. customThe zinc salts were then removed by filtration
  3. washthe residue washed with ethyl acetate
  4. extractionThe combined organic extract
  5. concentrationwas concentrated in vaccum
  6. dissolutionre-dissolved in CHCl3
  7. washwashed with NaHCO3, water and brine
  8. dry with materialFinally the organic layer was dried with Na2SO4 and solvent
  9. customevaporated

출처 및 근거

ORD 기록
ord-95652f6f54bc41bfbfaf4ba1f240c3dc
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157464B2

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