HRID553239

反应详情

EQUATION

反应方程式

HRID 553239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (88 mg, 0.46 mmol) and 1-hydroxybenzotriazole monohydrate (70 mg, 0.46 mmol) were added to a pyridine (2 ml) solution of the 4-(5-benzoylbenzimidazol-2-yl)-3,5-dimethylpyrrole-2-carboxylic acid (150 mg, 0.42 mmol) obtained in Example 10. N,N,N′-Trimethyl ethylenediamine (43 mg, 0.42 mmol) was added to the resultant solution and heated. The reaction mixture was stirred for 5 hours at 60° C. (internal temperature), and then allowed to cool to room temperature. The solvent was evaporated, and the residue was purified using medium pressure silica gel flash column chromatography (NH silica gel, chloroform:methanol=98:2) to afford N-methyl-N-(2-dimethylaminoethyl-4-(5-benzoylbenzimidazol-2-yl)-3,5-dimethylpyrrole-2-carboxamide (112 mg, 61%) as a light yellow amorphous.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto cool to room temperature
  3. customThe solvent was evaporated
  4. customthe residue was purified