Реакция #66609

ord-e4d2cf8e077f4252a86e82a5fa114462

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe vessel was capped
  2. 2
    ТемператураAfter 16 hours the solution was cooled to room temperature
  3. 3
    Другоеevaporated
  4. 4
    ЭкстракцияThe mixture was extracted with ethyl acetate
  5. 5
    Промывкаwashed with H2O
  6. 6
    Промывкаwashed with brine
  7. 7
    СушкаThe combined organic layers were dried over Na2SO4
  8. 8
    Фильтрацияfiltered
  9. 9
    Другоеevaporated in vacuo
  10. 10
    ДругоеPurification via flash chromatography (4:1 hexane/ethyl acetate)

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08524725B2uspto-grants-2013_09