HRID2411354

反应详情

EQUATION

反应方程式

HRID 2411354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-{5-bromo-2-[4-(3,5-dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}methanesulfonamide (634 mg) described in Preparation Example 226 was dissolved in N,N-dimethylformamide (5 mL), and sodium hydride (65.1 mg, 60% in oil) was added under ice-cooling. After stirring at room temperature for 10 min, methyl iodide (93 μL) was added, and the mixture was stirred overnight. To the reaction mixture was added water under ice-cooling, and the mixture was extracted with ethyl acetate. The solvent was evaporated under reduced pressure, and the residue was purified by column chromatography (ethyl acetate:hexane) to give the title compound (670 mg).

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture was stirred overnight
  3. temperaturecooling
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by column chromatography (ethyl acetate:hexane)