HRID59156

反应详情

EQUATION

反应方程式

HRID 59156 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-(4-methyl-1H-imidazol-1-yl)phenylamino)-6-(methoxymethyl)pyrimidin-4-yl)ethanone (160 mg, 0.44 mmol) in tetrahydrofuran (20 mL) was added dropwise to an ice-cold solution of methylmagnesium bromide (3.11 mL, 4.35 mmol) in tetrahydrofuran (10 mL). The mixture was stirred on ice-bath for 30 minutes and quenched with ammonium chloride (sat, aq). The mixture was extracted with dichloromethane, the organic phase was passed through a phase separator containing 1 cm layer of magnesium sulfate and the eluate was concentrated in vacuum. The residue was purified preparative HPLC to give the title compound as a solid, 124 mg (74%).

WORKUP

后处理

  1. customquenched with ammonium chloride (sat, aq)
  2. extractionThe mixture was extracted with dichloromethane
  3. additioncontaining 1 cm layer of magnesium sulfate
  4. concentrationthe eluate was concentrated in vacuum
  5. customThe residue was purified preparative HPLC