HRID59148

反应详情

EQUATION

反应方程式

HRID 59148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cold solution of methylmagnesium bromide (1.430 mL, 2.00 mmol) in THF (6 mL) a solution of 1-(6-(((3,3-difluorocyclobutyl)methoxy)methyl)-2-(3-methoxy-4-(6-methylpyridazin-4-yl)phenylamino)pyrimidin-4-yl)ethanone (94 mg, 0.20 mmol) in THF (3 mL) was added over 5 min. The mixture was stirred on ice-bath for 30 minutes before it was quenched with ammonium chloride (aq, sat). The solvent volume was reduced by evaporation. The mixture was extracted with dichloromethane and the organic phase was passed through a phase separator. The residue was purified by preparative HPLC to give the title compound as a dry film 38 mg (39%).

WORKUP

后处理

  1. customwas quenched with ammonium chloride (aq, sat)
  2. customThe solvent volume was reduced by evaporation
  3. extractionThe mixture was extracted with dichloromethane
  4. customThe residue was purified by preparative HPLC