Реакция #317380

ord-c2ef41a4d6934b76aa15a0b734f34a97

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture was heated
  2. 2
    Температураto reflux for three hours
  3. 3
    ДругоеThe reaction mixture was partitioned between water and ethyl acetate
  4. 4
    Другоеthe organic phase was separated
  5. 5
    Промывкаwashed with water
  6. 6
    Промывкаwashed with brine
  7. 7
    Сушкаdried (MgSO4)
  8. 8
    Фильтрацияfiltered
  9. 9
    Другоеevaporated under reduced pressure

Методика

4-Chloro-3-cyclopentyl-6-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine (500 mg, 1.860 mmol) was dissolved in 25 mL dry THF, and (S)-1-Amino-propan-2-ol (1.758 mL, 22.32 mmol) was added. The reaction mixture was heated to reflux for three hours, then cooled to room temperature. The reaction mixture was partitioned between water and ethyl acetate, and the organic phase was separated, washed with water, washed with brine, dried (MgSO4), filtered and evaporated under reduced pressure to give 0.56 g of (R)-1-(3-Cyclopentyl-6-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylamino)-propan-2-ol. Mass Spec. M+H=309.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07566708B2uspto-grants-2009_07