HRID2411235

反应详情

EQUATION

反应方程式

HRID 2411235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(5-Cyano-3-methylpyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (2.45 g) described in Preparation Example 102 was dissolved in dichloromethane (15 mL), trifluoroacetic acid (5 mL) was added, and the mixture was stirred at room temperature for 6 hr. The solvent was evaporated from the reaction mixture, aqueous potassium carbonate solution was added, and the mixture was extracted with chloroform. The solvent was evaporated from the organic layer, the obtained residue was purified by NH-coated silica gel silica gel column chromatography (hexane:ethyl acetate) to give the title compound (1.07 g).

WORKUP

后处理

  1. customThe solvent was evaporated from the reaction mixture, aqueous potassium carbonate solution
  2. additionwas added
  3. extractionthe mixture was extracted with chloroform
  4. customThe solvent was evaporated from the organic layer
  5. customthe obtained residue was purified by NH-coated silica gel silica gel column chromatography (hexane:ethyl acetate)