Reaktion #823501
ord-a13c16403f3a480798e28411e4943276
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeReaction mixture
- 2Waschenwashed with saturated NaHCO3 (3×20 mL)
- 3WaschenThe combined organic layers were washed with brine
- 4Trocknendried over Na2SO4
- 5Filtrationfiltered
- 6Einengenconcentrated in vacuo
- 7SonstigeThe crude product was purified by HPLC
Vorschrift
To a solution of 2,4-dichlorothieno[2,3-d]pyrimidine (805 mg, 3.94 mmol), TFA (0.91 mL, 11.82 mmol) in TFE (11 mL) was added 2,4,6-trimethylaniline (0.15 mg, 1.1 mmol) in a sealed tube. The reaction was stirred at 90° C. for 2 d. Reaction mixture was diluted with CH2Cl2 and washed with saturated NaHCO3 (3×20 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by HPLC to afford the product as a white solid (43.4 mg, 36%):