Reaktion #66609
ord-e4d2cf8e077f4252a86e82a5fa114462
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe vessel was capped
- 2TemperaturAfter 16 hours the solution was cooled to room temperature
- 3Sonstigeevaporated
- 4ExtraktionThe mixture was extracted with ethyl acetate
- 5Waschenwashed with H2O
- 6Waschenwashed with brine
- 7TrocknenThe combined organic layers were dried over Na2SO4
- 8Filtrationfiltered
- 9Sonstigeevaporated in vacuo
- 10SonstigePurification 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.