HRID456135

反应详情

EQUATION

反应方程式

HRID 456135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
127 °C

PROCEDURE

实验过程

To a degassed solution of 6-((6-bromo-1H-[1,2,3]triazolo[4,5-b]pyrazin-1-yl)methyl)quinoline (1.6 g, 4.69 mmol) in DMF (8 mL), was added Pd(PPh3)4 (0.434 g, 0.375 mmol) and dicyanozinc (0.441 g, 3.75 mmol). The reaction mixture was heated to 127° C. for 4 h. NH4Cl(aq) was added to quench the reaction, followed by EtOAc. The reaction mixture was filtered through celite, washed with saturated NaHCO3 and NH4Cl. The organic layer was separated, dried over Na2SO4, filtered and concentrated to give a crude product, which was purified with Analogix gel silica (Hexanes:EtOAc) to afford the title compound as a light yellow solid. LCMS (method B): [MH]+=288, tR=1.81 min.

WORKUP

后处理

  1. customto quench
  2. customthe reaction
  3. filtrationThe reaction mixture was filtered through celite
  4. washwashed with saturated NaHCO3 and NH4Cl
  5. customThe organic layer was separated
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give a crude product, which
  10. customwas purified with Analogix gel silica (Hexanes:EtOAc)