HRID59174

反应详情

EQUATION

反应方程式

HRID 59174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2-(3-Methoxy-4-(2-methyloxazol-5-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)methyl)-pyrimidin-4-yl)ethanone (64 mg, 0.15 mmol) was dissolved in THF (5 mL) and was added slowly to a solution of methylmagnesium bromide (3 M in THF, 0.391 mL, 1.17 mmol) in THF (5 mL). The mixture was stirred for 5 min. The mixture was cooled on ice bath and ammonium chloride (sat, aq, 5 mL) was added. The mixture was stirred for 5 min. The mixture was extracted with EtOAc (×2). The solvents were evaporated and the residue was purified by column chromatography eluting with a gradient of methanol in DCM to give the title compound as a solid, 46 mg (69%).

WORKUP

后处理

  1. temperatureThe mixture was cooled on ice bath
  2. stirringThe mixture was stirred for 5 min
  3. extractionThe mixture was extracted with EtOAc (×2)
  4. customThe solvents were evaporated
  5. customthe residue was purified by column chromatography
  6. washeluting with a gradient of methanol in DCM