HRID2411863

反应详情

EQUATION

反应方程式

HRID 2411863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of (4-bromo-2-fluorophenyl)[4-(3,5-dimethylpyridin-2-yl)piperazin-1-yl]methanone (157 mg) described in Preparation Example 114, 1-benzoyl-5-methylimidazolidin-2-one (105 mg) described in Preparation Example 56, tripotassium phosphate (170 mg) and copper(I) iodide (76 mg) were added 1,4-dioxane (8 mL) and N,N′-dimethylethylenediamine (86 μL), and the mixture was stirred with heating under reflux for 10 hr. The reaction mixture was cooled, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over sodium sulfate, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (35 mg).

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for 10 hr
  3. temperatureThe reaction mixture was cooled
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over sodium sulfate
  7. customthe solvent was evaporated
  8. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)