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

HRID 1372020
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1372020
[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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 176Acetic AcidLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-95652f6f54bc41bfbfaf4ba1f240c3dc
Quelldatensatz
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07157464B2

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