Reaktion #78468

ord-33fe644023524c8aa8fe79dfb685ac47

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe catalyst was then filtered off
  2. 2
    workup.DISTILLATIONthe solvent was distilled off in vacuo
  3. 3
    SonstigeThe crude oily product obtained
  4. 4
    Sonstigewas further reacted directly

Vorschrift

To a solution of 3.1 g (15 mmol) of methyl 6-methylamino-5-nitronicotinate in 100 mL of ethanol/dichloromethane (3:1) was added 1 g of palladium on charcoal (10%) and the resulting suspension was hydrogenated at room temperature under 5 bar of hydrogen pressure for 1.5 hours. The catalyst was then filtered off and the solvent was distilled off in vacuo. The crude oily product obtained was further reacted directly. Yield: 2.4 g (92% of theory); Rf value: 0.44 (silica gel; ethyl acetate/ethanol/ammonia=90:10:1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06710055B2uspto-grants-2004_03