HRID1072934

反应详情

EQUATION

反应方程式

HRID 1072934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In the same manner as in Example 1, N,N′-carbonyldiimidazole (0.290 g) was added to a mixture of 6-carboxy-1-(2,4-dichlorobenzyl)-3-methyl-2-benzimidazolone (0.314 g) and N,N-dimethylformamide (9 ml), and the mixture was stirred at room temperature for 1 hr. 1-n-Butanesulfonamide (0.246 g) and DBU (0.273 g) were added and the mixture was stirred at 100° C. for 16 hr. The solvent was evaporated and the resulting mixture was extracted with chloroform and water. The organic layer was concentrated and the residue was purified by preparative thin layer chromatography to give 6-(1-n-butanesulfonylcarbamoyl)-1-(2,4-dichlorobenzyl)-3-methyl-2-benzimidazolone (0.123 g).

WORKUP

后处理

  1. stirringthe mixture was stirred at 100° C. for 16 hr
  2. customThe solvent was evaporated
  3. extractionthe resulting mixture was extracted with chloroform and water
  4. concentrationThe organic layer was concentrated
  5. customthe residue was purified by preparative thin layer chromatography