Reaktion #79784

ord-b977410907254daabd8a9c7bcaa27135

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.STIRRINGThe mixture was stirred at ambient temperature for 1 hour
  2. 2
    Sonstigeevaporated under vacuum
  3. 3
    SonstigeThe residue was partitioned between water and ethyl acetate
  4. 4
    SonstigeThe ethyl acetate was separated
  5. 5
    Sonstigedried
  6. 6
    Sonstigeevaporated
  7. 7
    Sonstigethe residue obtained
  8. 8
    Sonstigewas recrystallised from toluene

Vorschrift

Isobutyryl chloride (1.8 g) was added dropwise to a mixture of 5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine (4.32 g), dry dimethyl-formamide (200 ml) and dry pyridine (2 ml) with stirring under nitrogen at 20° C. The mixture was stirred at ambient temperature for 1 hour and evaporated under vacuum. The residue was partitioned between water and ethyl acetate. The ethyl acetate was separated, dried and evaporated and the residue obtained was recrystallised from toluene to give 7-isobutyryl-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine, m.p. 160.5-161° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713474B2uspto-grants-2004_03