HRID2412004

反应详情

EQUATION

反应方程式

HRID 2412004 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 1-{5-chloro-2-[4-(3,5-dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}-3-methylimidazolidin-2-one (116 mg) described in Preparation Example 241, pyrrolidin-2-one (35 mg), tripotassium phosphate (81 mg), tris(dibenzylideneacetone)dipalladium(0)-chloroform adduct (28 mg) and 2-di-tert-butylphosphino-3,4,5,6-tetramethyl-2′,4′,6′-triisopropyl-1,1′-biphenyl (13 mg) was added tert-butanol (1.5 mL), and the mixture was stirred with heating under reflux for 8 hr. After cooling, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The solvent was evaporated, and the residue was purified by column chromatography (ethyl acetate:methanol) to give the title compound (62 mg).

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for 8 hr
  3. temperatureAfter cooling
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe solvent was evaporated
  6. customthe residue was purified by column chromatography (ethyl acetate:methanol)