HRID1042290

反应详情

EQUATION

反应方程式

HRID 1042290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-chloro-6-methylisoquinolin-5-amine (414 mg, 2147 μmol) and 4-(2-fluoropyridin-3-yl)-1H-pyrazolo[3,4-d]pyrimidine (420 mg, 1952 μmol) in THF (20 ml) was sonicated until all solid became a fine powder. Lithium bis(trimethylsilyl)amide, 1.0 M solution in THF (6831 μl, 6831 mmol) was then added (all solids were dissolved and color changed) The mixture was stirred at rt overnight. The mixture was poured into a mixture of MeOH (20 ml) and AcOH (2 ml) and then solvent was removed in vacuo. 2 M NH3/MeOH (30 ml) was added and then solvent was removed in vacuo. The product was purified by flash chromatography eluting with MeOH/DCM (0-5%) to give N-(3-(1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-yl)-1-chloro-6-methylisoquinolin-5-amine. MS Found (ESI pos. ion) m/z 388 (M+H+).

WORKUP

后处理

  1. customwas sonicated until all solid
  2. dissolutionwere dissolved
  3. customsolvent was removed in vacuo
  4. addition2 M NH3/MeOH (30 ml) was added
  5. customsolvent was removed in vacuo
  6. customThe product was purified by flash chromatography
  7. washeluting with MeOH/DCM (0-5%)