Reaktion #2353255

ord-4c11b9bc7650413fa673f1780d7f4b5a

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe vessel was capped
  2. 2
    TemperaturAfter 16 hours the solution was cooled to room temperature
  3. 3
    Sonstigeevaporated
  4. 4
    ExtraktionThe mixture was extracted with ethyl acetate
  5. 5
    Waschenwashed with H2O
  6. 6
    Waschenwashed with brine
  7. 7
    TrocknenThe combined organic layers were dried over Na2SO4
  8. 8
    Filtrationfiltered
  9. 9
    Sonstigeevaporated in vacuo
  10. 10
    SonstigePurification via flash chromatography (4:1 hexane/ethyl acetate)

Vorschrift

To a glass pressure vessel containing 4-chloro-5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methylsulfanyl-pyrimidine (0.212 g, 0.6 mmol) was added 5.0 mL ethyl amine via a cold finger condenser. The vessel was capped and warmed to 50° C. After 16 hours the solution was cooled to room temperature, evaporated and taken up in H2O. The mixture was extracted with ethyl acetate, washed with H2O and then washed with brine. The combined organic layers were dried over Na2SO4, filtered and evaporated in vacuo. Purification via flash chromatography (4:1 hexane/ethyl acetate) afforded ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methylsulfanyl-pyrimidin-4-yl]-amine (0.136 g, 63%) as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07858632B2uspto-grants-2010_12