HRID629036

反应详情

EQUATION

反应方程式

HRID 629036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(4-chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenylamine (200 mg, 0.594 mmol.), morpholin (103 mg, 1.118 mmol, 2.0 eq), triethylamine (120 mg, 1.118 mmol, 2.0 eq) in dioxane (8 ml) and the mixture was reacted for 16 hrs at 90° C. The reaction mixture was dried and the solvent was removed by evaporation in vacuo. The reaction mixture was partitioned between EA and water. The organic layer was washed with brine, dried over MgSO4, filtered and evaporated in vacuo. The resulting residue was purified using flash chromatography on silica gel (EA), and recrystallized by (Hexane/EtOAc) to give a gray white 106 mg (46.1%).

WORKUP

后处理

  1. customthe mixture was reacted for 16 hrs at 90° C
  2. customThe reaction mixture was dried
  3. customthe solvent was removed by evaporation in vacuo
  4. customThe reaction mixture was partitioned between EA and water
  5. washThe organic layer was washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customThe resulting residue was purified
  10. customrecrystallized by (Hexane/EtOAc)
  11. customto give a gray white 106 mg (46.1%)