HRID1181669

反应详情

EQUATION

反应方程式

HRID 1181669 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a flask was added 50 mL of 2N hydrochloric acid, and powdery phthalimide (7.4 g, 0.05 mol) was slowly added thereto with stirring. Then, the mixture was stirred at 97° C. for 3 hours to obtain an aqueous solution containing phthalic acid. Phthalic acid was recovered by condensing and filtering the aqueous solution. Then, to a flask, were added the phthalic acid, 100 mL of pyridine and 0.5 g of sulfuric acid, and stirred for 3 hours at 100° C. with distilling off water formed by reaction to obtain a mixture containing phthalic anhydride. Hydroxylamine hydrochloride NH2OH.HCl (6.9 g, 0.1 mol) was added to the mixture and stirred at 50° C. for 3 hour to form N-hydroxyphthalimide (5.74 g, yield 70%).

WORKUP

后处理

  1. additionwas slowly added
  2. stirringThen, the mixture was stirred at 97° C. for 3 hours
  3. customto obtain an aqueous solution
  4. customPhthalic acid was recovered by condensing
  5. filtrationfiltering the aqueous solution
  6. additionThen, to a flask, were added the phthalic acid, 100 mL of pyridine and 0.5 g of sulfuric acid
  7. stirringstirred for 3 hours at 100° C.
  8. distillationwith distilling off water
  9. customformed by reaction
  10. customto obtain a mixture
  11. stirringstirred at 50° C. for 3 hour