HRID730022
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheat to reflux
- temperaturereflux for 1 h
- filtrationFilter while slurry
- filtrationFilter off solids
- washwash 2×100 mL water
- customdry under reduced pressure at 45-50° C.