HRID1175371

反应详情

EQUATION

反应方程式

HRID 1175371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The title compound was prepared according to the procedure outlined in example 1 step (iv) using a mixture of 1-methyl-1H-imidazole-4-sulfonamide (0.25 g), tris(dibenzylideneacetone)dipalladium (0) (0.10 g), 2-dicyclohexylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (XPHOS) (60 mg), cesium carbonate (0.26 g), 4-chloro-6-(difluoromethoxy)-2-[[(2,3-difluorophenyl)methyl]thio]-pyrimidine (product of example 12, step ii) (0.18 g) and anhydrous dioxane (5 ml). Purification was by tituration with methanol/DCM. The resulting white solid was diluted with H2O and extracted with EtOAc. The organic layer was washed with H2O (×2) then brine and dried (MgSO4), filtered and evaporated. The resulting oil was triturated with methanol/DCM to give the title compound as a white solid. Yield: 15 mg

WORKUP

后处理

  1. customThe title compound was prepared
  2. customPurification
  3. additionThe resulting white solid was diluted with H2O
  4. extractionextracted with EtOAc
  5. washThe organic layer was washed with H2O (×2)
  6. dry with materialbrine and dried (MgSO4)
  7. filtrationfiltered
  8. customevaporated
  9. customThe resulting oil was triturated with methanol/DCM