HRID335287

反应详情

EQUATION

反应方程式

HRID 335287 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethyl 3-(3-(5-(3,4-difluorobenzylcarbamoyl)-2-fluorophenylcarbamoyl)imidazo[1,2-a]pyridin-7-yl)propanoate (step 1) (50 mg, 0.095 mmol) was suspended in dry ether and cooled to 0° C. Methylmagnesium bromide (0.318 ml, 3.0M in ether, 0.953 mmol) was added and the mixture was stirred and allowed to warm to RT over 16 hrs. The mixture was partitioned between 10% aq. Citric acid and EtOAc. The organics were separated, dried (MgSO4), filtered and evaporated to dryness. The residue was purified by chromatography on silica eluting with 0-10% MeOH in DCM to afford the title product;

WORKUP

后处理

  1. temperatureto warm to RT over 16 hrs
  2. customThe mixture was partitioned between 10% aq. Citric acid and EtOAc
  3. customThe organics were separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe residue was purified by chromatography on silica eluting with 0-10% MeOH in DCM