Reaktion #684651

ord-c4cabf65134f4e46bd0e4cd78c0d77de

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONare added dropwise at -20° C
  2. 2
    Einengenconcentrated
  3. 3
    Extraktionextracted with ether
  4. 4
    Sonstigeevaporated
  5. 5
    SonstigeThe product is purified by adsorption chromatography on silica gel by elution with benzene

Vorschrift

20.2 g (0.2 mole) of triethylamine are added to 47.2 g (0.2 mole) of 2,4-dichloro-5-nitro-6-isopropyl-pyridine in 1 liter of ethanol and 17.5 g (0.2 mole) of 3-aminopentane are added dropwise at -20° C. The reaction mixture is stirred overnight at 20° C and then concentrated. The residue is suspended in water and extracted with ether. The ethereal extracts are drid over MgSO4 and evaporated. The product is purified by adsorption chromatography on silica gel by elution with benzene to yield 48 g of 2-chloro-4-(3-pentylamino-5-nitro-6-isopropyl-pyrimidine (nD20 : 1.5478).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04014677uspto-grants-1977_03