HRID622295

反应详情

EQUATION

反应方程式

HRID 622295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-2-fluoro-5-nitroaniline (19 g) and 3,4,5,6-tetrahydrophthalic anhydride (15.2 g) were dissolved in acetic acid (50 ml) and refluxed for 6 hours. After being allowed to cool, the resultant mixture was poured into water and extracted with toluene. The toluene layer was washed with water, an aqueous sodium hydrogen carbonate solution and water in order, dried and concentrated. The residue was crystallized from ethanol to give 20 g of N-(4-chloro-2-fluoro-5-nitrophenyl)-3,4,5,6-tetrahydrophthalimide. M.P., 157°-157.5° C.

WORKUP

后处理

  1. temperaturerefluxed for 6 hours
  2. temperatureto cool
  3. extractionextracted with toluene
  4. washThe toluene layer was washed with water
  5. dry with materialan aqueous sodium hydrogen carbonate solution and water in order, dried
  6. concentrationconcentrated
  7. customThe residue was crystallized from ethanol