HRID32523

反应详情

EQUATION

反应方程式

HRID 32523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

m-CPBA (70-75%, 105 mg) was added to a stirred solution of 6-(1-methyl-4-phenyl-1H-imidazol-5-yl)-4-(methylthio)thieno[2,3-d]pyrimidine (example 7) (72 mg) in DCM (5 mL), stirred for 6 hours then 2M Na2S2O3 (2.5 mL) was added. The organic layer was separated and the aqueous layer extracted with DCM (2×15 mL). The combined organics were washed with saturated aqueous NaHCO3 (10 mL), dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluting with hexane:EtOAc (1:4) afforded the title compound as a yellow solid (44 mg, 56%);

WORKUP

后处理

  1. customThe organic layer was separated
  2. extractionthe aqueous layer extracted with DCM (2×15 mL)
  3. washThe combined organics were washed with saturated aqueous NaHCO3 (10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customPurification by flash chromatography on silica eluting with hexane:EtOAc (1:4)