HRID32645

反应详情

EQUATION

反应方程式

HRID 32645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzylchloroformate (0.027 mL) was added to a solution of 6-[4-(3-aminophenyl)-1-methyl-1H-imidazol-5-yl]thieno[2,3-d]pyrimidin-4-amine (Intermediate 110) (40 mg) and pyridine (0.02 mL) in THF (7 mL). The mixture was stirred under an inert atmosphere for 1 hour, then quenched with H2O (10 mL) and extracted EtOAc (3×10 mL). The combined organics were dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluting with CH2Cl2:MeOH (0-10%) gave the title compound as a gum (16 mg, 28%);

WORKUP

后处理

  1. customquenched with H2O (10 mL)
  2. extractionextracted EtOAc (3×10 mL)
  3. dry with materialThe combined organics were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurification by flash chromatography on silica eluting with CH2Cl2