HRID2411249

反应详情

EQUATION

反应方程式

HRID 2411249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(3,5-Dimethylpyridin-2-yl)piperazine (3.8 g) described in Preparation Example 79 and 4-bromo-2-methylbenzoic acid (4.3 g) were dissolved in a solution of chloroform (30 mL) and methanol (30 mL), 4-(4,6-dimethoxy[1.3.5]triazin-2-yl)-4-methylmorpholinium chloride hydrate (DMT-MM) (8.8 g) was added, and the mixture was stirred at room temperature overnight. The solvent was evaporated from the reaction mixture, ethyl acetate was added, and the insoluble material was collected by filtration. The solvent was evaporated from the obtained filtrate, and the residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (7 g).

WORKUP

后处理

  1. additionwas added
  2. customThe solvent was evaporated from the reaction mixture, ethyl acetate
  3. additionwas added
  4. filtrationthe insoluble material was collected by filtration
  5. customThe solvent was evaporated from the obtained filtrate
  6. customthe residue was purified by column chromatography (hexane:ethyl acetate)