Reaktion #79784
ord-b977410907254daabd8a9c7bcaa27135
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.STIRRINGThe mixture was stirred at ambient temperature for 1 hour
- 2Sonstigeevaporated under vacuum
- 3SonstigeThe residue was partitioned between water and ethyl acetate
- 4SonstigeThe ethyl acetate was separated
- 5Sonstigedried
- 6Sonstigeevaporated
- 7Sonstigethe residue obtained
- 8Sonstigewas 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.