HRID1974036

反应详情

EQUATION

反应方程式

HRID 1974036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1-hydroxy-6-chloro-2-(trifluoromethyl)-1H-imidazo(4,5-b)pyridine (2.37 grams) in 5 milliliters of pyridine was added octanoyl chloride (1.63 grams). The addition was carried out portionwise with stirring and resulted in the precipitation of a white solid. The reaction mixture was set on a steam bath for twenty minutes, then poured over ice cold aqueous HCl. An oil separated and subsequently crystallized on vigorous stirring. This precipitate was removed by filtration, dissolved in ether, dried over magnesium sulfate, filtered, and ether removed by evaporation under vacuum. The substance was purified by distillation, m.p., 33.5°-35.5° C.

WORKUP

后处理

  1. additionThe addition
  2. customresulted in the precipitation of a white solid
  3. waitThe reaction mixture was set on a steam bath for twenty minutes
  4. additionpoured over ice cold aqueous HCl
  5. customAn oil separated
  6. customsubsequently crystallized on vigorous stirring
  7. customThis precipitate was removed by filtration
  8. dissolutiondissolved in ether
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. customether removed by evaporation under vacuum
  12. distillationThe substance was purified by distillation
  13. customm.p., 33.5°-35.5° C.