HRID565130

反应详情

EQUATION

反应方程式

HRID 565130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 30 ml of pyridine, 2.4 g of the compound (2) obtained in Example 2 were dissolved. Under ice cooling and stirring, 2.9 g of the compound (1) obtained in Example 1 were added in small portions. Subsequent to stirring at room temperature for 2 hours, the pyridine was distilled off under reduced pressure. CHCl3 was added further, and distillation was repeated twice under reduced pressure. The residue was isolated and purified by chromatography on a silica gel column (eluent: CHCl3), whereby 2.7 g of the compound (3) were obtained (yield: 54%).

WORKUP

后处理

  1. stirringSubsequent to stirring at room temperature for 2 hours
  2. distillationthe pyridine was distilled off under reduced pressure
  3. additionCHCl3 was added further
  4. distillationdistillation
  5. customThe residue was isolated
  6. custompurified by chromatography on a silica gel column (eluent: CHCl3)