Reaktion #823501

ord-a13c16403f3a480798e28411e4943276

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeReaction mixture
  2. 2
    Waschenwashed with saturated NaHCO3 (3×20 mL)
  3. 3
    WaschenThe combined organic layers were washed with brine
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo
  7. 7
    SonstigeThe 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%):

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07595324B2uspto-grants-2009_09