Triethylamine → 1-tert-Butyl-3-methyl-1H-pyrazol-5-amine

HRID 1466208

Reaktionsgleichung

Reaktionsgleichung von HRID 1466208
N[C:2]([CH3:6])=[CH:3][C:4]#[N:5].[C:7]([NH:11][NH2:12])([CH3:10])([CH3:9])[CH3:8].C(N(CC)CC)C>C(O)C>[C:7]([N:11]1[C:4]([NH2:5])=[CH:3][C:2]([CH3:6])=[N:12]1)([CH3:10])([CH3:9])[CH3:8]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 706993-Amino-2-butenenitrileHCID 81890tert-Butylhydrazine

Produkt 1

HCID 7372001-tert-Butyl-3-methyl-1H-pyrazol-5-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a mixture of 3-aminobut-2-enenitrile (60 g, 731 mmol) and tert-butylhydrazine (96 g, 731.1 mmol) in ethanol (35 ml), triethylamine (220 ml, 2195 mmol) was added. The mixture was refluxed for 12-16 h. The reaction mixture was then concentrated under reduced pressure. The concentrate was extracted with water (100 ml) and ethylacetate (700 ml). The organic layer was washed with brine and dried over Na2SO4 and concentrated under reduced pressure to obtain the title product.

Aufarbeitung

  1. additionwas added
  2. temperatureThe mixture was refluxed for 12-16 h
  3. concentrationThe reaction mixture was then concentrated under reduced pressure
  4. extractionThe concentrate was extracted with water (100 ml) and ethylacetate (700 ml)
  5. washThe organic layer was washed with brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c2761e0481744b4c8ce5b257eb2263c8
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09000007B2

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