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Piperazine → N-(2-Cyclobutylethyl)-6-(1-piperazinyl)-3-pyridazinecarboxamide

HRID 2354630
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2354630
[CH:1]1([CH2:5][CH2:6][NH:7][C:8]([C:10]2[N:11]=[N:12][C:13](Cl)=[CH:14][CH:15]=2)=[O:9])[CH2:4][CH2:3][CH2:2]1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C(#N)C>[CH:1]1([CH2:5][CH2:6][NH:7][C:8]([C:10]2[N:11]=[N:12][C:13]([N:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)=[CH:14][CH:15]=2)=[O:9])[CH2:4][CH2:3][CH2:2]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 4837PiperazineHCID 860260456-CHLOROPYRIDAZINE-3-CARBOXYLIC Acid (2-CYCLOBUTYLETHYL)AMIDE

Produkt 1

HCID 66849365N-(2-Cyclobutylethyl)-6-(1-piperazinyl)-3-pyridazinecarboxamideAusbeute 78,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 6-chloropyridazine-3-carboxylic acid (2-cyclobutylethyl)-amide (1.2 g, 5.00 mmol) in acetonitrile (40 mL) was added piperazine (1.29 g, 15.00 mmol). The reaction mixture was heated to reflux overnight. The mixture was evaporated and the solid residue was taken in ethyl acetate (100 mL) and water (100 mL). The organic layer was separated and the aqueous layer was extracted with ethyl acetate (2×100 mL). The combined ethyl acetates were dried over Na2SO4 and concentrated in vacuo to give the title compound as yellow solid (1.14 g, 78.4% yield).

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux overnight
  3. customThe mixture was evaporated
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with ethyl acetate (2×100 mL)
  6. dry with materialThe combined ethyl acetates were dried over Na2SO4
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a6d4f9a2cd9745978039afbbc6c2708b
Quelldatensatz
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07754711B2

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