HRID259570

反应详情

EQUATION

反应方程式

HRID 259570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ten grams of 4-(cyanomethyl)benzoic acid is refluxed in 70 mls. of thionyl chloride for four hours. The solvents are removed leaving a residue of 4-cyanomethylbenzoyl chloride. To a solution of 5.5 g. of 3-amino-2-hydroxy pyridine in cold pyridine there is added slowly, with cooling, 8 g. of 4-cyanomethyl benzoyl chloride. The mixture is allowed to come to room temperature and stirred overnight. The mixture is added to 300 ml. of ice and the solid amide separated by filtration and recrystallized from methanol. A mixture of 3 g. of the above amide in 50 mls. of phosphorus oxychloride is heated under reflux for 5 hours. The solvents are removed in vacuo and the residue is crystallized from ethyl acetate to give 2-(4-cyanomethylphenyl)oxazolo[5,4-b]pyridine.

WORKUP

后处理

  1. temperaturewith cooling
  2. customto come to room temperature
  3. additionThe mixture is added to 300 ml
  4. customof ice and the solid amide separated by filtration
  5. customrecrystallized from methanol
  6. additionA mixture of 3 g
  7. temperatureof phosphorus oxychloride is heated
  8. temperatureunder reflux for 5 hours
  9. customThe solvents are removed in vacuo
  10. customthe residue is crystallized from ethyl acetate