HRID17847

反应详情

EQUATION

反应方程式

HRID 17847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-fluoro-3-sulphamoylbenzoic acid (5.4 mmol) in thionyl chloride (10 mL) is refluxed for 4 hours. The reagent is then removed by distillation under reduced pressure and the residue is re-dissolved in dry toluene (10 mL). The solvent is removed by distillation under reduced pressure. This operation is repeated twice, and then the residue is dissolved in dry dioxane (10 mL), and ammonia (6 mmol) and pyridine (6 mmol) are added. After one hour, the solvent is removed under reduced pressure and the residue is taken up in methanol (5 mL), and then water (30 mL) is added. The precipitate obtained is collected by filtration, washed with water and dried.

WORKUP

后处理

  1. customThe reagent is then removed by distillation under reduced pressure
  2. dissolutionthe residue is re-dissolved in dry toluene (10 mL)
  3. customThe solvent is removed by distillation under reduced pressure
  4. dissolutionthe residue is dissolved in dry dioxane (10 mL)
  5. customthe solvent is removed under reduced pressure
  6. additionwater (30 mL) is added
  7. customThe precipitate obtained
  8. filtrationis collected by filtration
  9. washwashed with water
  10. customdried