HRID274571

反应详情

EQUATION

反应方程式

HRID 274571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 2-butyl-1-[[4-(2-cyanobenzo[b]furan-3-yl)phenyl]methyl]benzimidazole-7-carboxylate (1.3 g) and trimethyltin azide (2.9 g) in toluene (125 ml) was heated under reflux for 2 days. After concentration to dryness, the residue was dissolved in a mixture of methanol (150 ml) and 1N hydrochloric acid (25 ml) and the mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated to dryness and the residue was dissolved in methylene chloride. The resulting solution was washed with water, dried and concentrated to dryness. The residue was purified by column chromatography on silica gel to give pale yellow powders (1.3 g).

WORKUP

后处理

  1. temperatureunder reflux for 2 days
  2. concentrationAfter concentration to dryness
  3. dissolutionthe residue was dissolved in a mixture of methanol (150 ml) and 1N hydrochloric acid (25 ml)
  4. concentrationThe reaction mixture was concentrated to dryness
  5. dissolutionthe residue was dissolved in methylene chloride
  6. washThe resulting solution was washed with water
  7. customdried
  8. concentrationconcentrated to dryness
  9. customThe residue was purified by column chromatography on silica gel