Реакция #325192

ord-72a5b2157406494fad0a968383749c43

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеreaction
  2. 2
    Другоеreaction
  3. 3
    workup.STIRRINGwas stirred for 2 hours
  4. 4
    ДругоеSolid K2CO3 was removed by filtration
  5. 5
    ДругоеSolvent was partially removed in vacuo
  6. 6
    workup.ADDITIONSodium citrate (50 ml) was added
  7. 7
    Другоеreaction
  8. 8
    Экстракцияwas extracted with EtOAc
  9. 9
    КонцентрированиеOrganic phases concentrated in vacuo
  10. 10
    Другоеpurified
  11. 11
    Другоеto yield BA79

Методика

3-(3-fluoro-5-methoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (BA75, 100 mg, 0.386 mmol) was dissolved in DMF (10 ml). K2CO3 (250 mg, 1.54 mmol) was added and reaction was stirred at room temperature under an argon atmosphere. Iodocyclopentane (0.134 ml, 1.16 mmol) was added with a syringe and reaction was stirred for 2 hours. Solid K2CO3 was removed by filtration. Solvent was partially removed in vacuo. Sodium citrate (50 ml) was added and reaction was extracted with EtOAc. Organic phases concentrated in vacuo and purified using by RP-HPLC (MeCN:H2O:0.1% TFA) to yield BA79.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08642604B2uspto-grants-2014_02