HRID2218396

反应详情

EQUATION

反应方程式

HRID 2218396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

6,7-Dichloro-2-[4-(2-morpholin-4-ylethoxy)phenyl]-3H-imidazo[4,5-b]pyridine (Example 206) (0.10 g, 0.25 mmol), benzyl mercaptan (0.036 ml, 0.3 mmol) and potassum tert-butanolate (0.071 g, 0.63 mmol) were dissolved in DMF (1 ml) and heated to 80° C. for 48 h. The reaction mixture was diluted with EtOAc and extracted with 2M HCl. The aqueous phase was basified with 10M NaOH and extracted with EtOAc. The organic phase was dried (Na2SO4) and evaporated in vacuo and the residue was dissolved in CH3CN (3 ml) and purified by HPLC-C18, giving the title product as a bis(trifluoroacetate) (37%).

WORKUP

后处理

  1. extractionextracted with 2M HCl
  2. extractionextracted with EtOAc
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. customevaporated in vacuo
  5. dissolutionthe residue was dissolved in CH3CN (3 ml)
  6. custompurified by HPLC-C18