HRID1817046

反应详情

EQUATION

反应方程式

HRID 1817046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(pentan-3-yl)-6-((trimethylsilyl)ethynyl)-1H-imidazo[4,5-b]pyrazin-2-ol (3.2 g, 10.6 mmol), KF (1.6 g, 27.5 mmol) in MeOH/THF/H2O (50 mL, 2/2/1) was stirred at room temperature. Upon complete conversion by LCMS, the solution was concentrated in vacuo, diluted with EtOAc, washed with NH4Cl solution, dried over Na2SO4, and concentrated in vacuo. Purification over silica gel (Biotage MPLC 10-80% EtOAc/Hexanes) gave a brown solid, which was washed with 15% EtOAc/hexanes to give product the title compound as a white solid (0.9 g, 37%).

WORKUP

后处理

  1. concentrationUpon complete conversion by LCMS, the solution was concentrated in vacuo
  2. additiondiluted with EtOAc
  3. washwashed with NH4Cl solution
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customPurification over silica gel (Biotage MPLC 10-80% EtOAc/Hexanes)
  7. customgave a brown solid, which
  8. washwas washed with 15% EtOAc/hexanes