HRID2235564

反应详情

EQUATION

反应方程式

HRID 2235564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.73 g (11.6 mmol) of 3-methyl-1,3-dihydroimidazo[4,5-c]pyridin-2-one in 6.3 mL of concentrated sulfuric acid, cooled in an 0° C. ice bath, was slowly added a solution of 1.50 mL (36.0 mmol) of fuming nitric acid in 1.5 mL of concentrated sulfuric acid. The reaction was removed from the ice bath and stirred for 0.5 h at room temperature and then heated at 100° C. for 2 h. The reaction was quenched over 300 mL of ice and solid ammonium carbonate was added to adjust the pH to 9. The resulting slurry was filtered and the collected solids washed with water and dried under high vacuum to give 1.94 g (86%) of the title compound.

WORKUP

后处理

  1. customThe reaction was removed from the ice bath
  2. temperatureheated at 100° C. for 2 h
  3. customThe reaction was quenched over 300 mL of ice and solid ammonium carbonate
  4. additionwas added
  5. filtrationThe resulting slurry was filtered
  6. washthe collected solids washed with water
  7. customdried under high vacuum