HRID2073800

反应详情

EQUATION

反应方程式

HRID 2073800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8-amino-3-(2-propynyl)-2-methylimidazo[1,2-a]pyridine (8.0 g) and triethylamine (4.8 g) in methanol (80 ml) was added 2-methyl-6-methoxycarbonylaminobenzyl chloride (10.15 g) and the mixture was stirred at room temperature for 17 hours. After methanol was evaporated in vacuo, the resultant residue was dissolved in methylene chloride (100 ml) and the mixture was washed with water and dried over magnesium sulfate. The solvent was evaporated in vacuo. The resultant residue was subjected to column chromatography on silica gel (240 g) and eluted with a mixture of chloroform and ethyl acetate (20:1) to give a crystalline product. The crystals were recrystallized from a mixture of ethyl acetate and n-hexane to give 8-(2-methyl-6-methoxycarbonylaminobenzylamino)-3-(2-propynyl)-2-methylimidazo[1,2-a]pyridine (6.08 g).

WORKUP

后处理

  1. customAfter methanol was evaporated in vacuo
  2. dissolutionthe resultant residue was dissolved in methylene chloride (100 ml)
  3. washthe mixture was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated in vacuo
  6. washeluted with a mixture of chloroform and ethyl acetate (20:1)
  7. customto give a crystalline product
  8. customThe crystals were recrystallized from a mixture of ethyl acetate and n-hexane