HRID730022

反应详情

EQUATION

反应方程式

HRID 730022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add methanol (1,200 mL) to combined lots of 3-(2,2-dimethyl-propyl)-5-(4-fluoro-phenylethynyl)-3H-imidazo[4,5-b]pyridin-2-ylamine (37.30 g) and heat to reflux. Add activated charcoal (3.73 g, 10 wt %) and reflux for 1 h. Filter while slurry is hot, then add water (375 mL) to the filtrate with stirring at room temperature. Filter off solids, wash 2×100 mL water and dry under reduced pressure at 45-50° C. to provide 30.0 g (80%) of the desired compound.

WORKUP

后处理

  1. temperatureheat to reflux
  2. temperaturereflux for 1 h
  3. filtrationFilter while slurry
  4. filtrationFilter off solids
  5. washwash 2×100 mL water
  6. customdry under reduced pressure at 45-50° C.