HRID1066158

反应详情

EQUATION

反应方程式

HRID 1066158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Amino-3-sulfamoylbenzoic acid (6 g) and thiocarbonyldiimidazole (23.2 g) in dioxane (60 mL) was refluxed for 2 h. The solvent was removed by distillation under reduced pressure. The residue was dispersed in water (200 mL) and supplemented with a 10% aqueous solution of NaOH (40 mL). After stirring for 30 min. at room temperature, the solution was treated with charcoal, filtered, and the filtrate was adjusted to pH 2 with 12N HCl. The resulting precipitate was collected by filtration, washed with water and dried to give the title compound (yield: 4.5 g); m.p. >300° C.

WORKUP

后处理

  1. customThe solvent was removed by distillation under reduced pressure
  2. additionThe residue was dispersed in water (200 mL)
  3. additionthe solution was treated with charcoal
  4. filtrationfiltered
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with water
  7. customdried