Reaktion #460190

ord-ae92bd6dddcb469380f01c14b37b72bc

Reaktionsgleichung

[BH4-].[Na+]
sodium borohydride
O=[N+]([O-])c1cnn(CCCCN2CCN(c3ncccn3)CC2)c1
4-nitro-1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole
CCC(C)=O
methyl ethyl ketone
CCC(C)Nc1cnn(CCCCN2CCN(c3ncccn3)CC2)c1
4-(2-butyl)amino-1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThis temperature is maintained for 30 minutes
  2. 2
    Sonstigeto rise to room temperature
  3. 3
    Sonstigethe mixture is evaporated under vacuum
  4. 4
    Sonstigeare obtained in liquid form

Vorschrift

0.9 g (24 mmol) of sodium borohydride is added to a suspension, cooled to 0° C., of 2.8 g (12 mmol) of nickel dichloride hexahydrate in a solution of 2 g (6 mmol) of 4-nitro-1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole, Example 7, and 10 ml of methyl ethyl ketone in 50 ml of ethanol. This temperature is maintained for 30 minutes and allowed to rise to room temperature, stirring is continued for 2 hours, the mixture is evaporated under vacuum, the residue is taken up with ethyl acetate and 1.22 g of 4-(2-butyl))amino-1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole are obtained in liquid form.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05162323uspto-grants-1992_11