HRID2189803

反应详情

EQUATION

反应方程式

HRID 2189803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 5-(5-{5-chloro-6-[(1-methylethyl)oxy]-3-pyridinyl}-1,2,4-oxadiazol-3-yl)-1H-indazole (D110) (335 mg, 0.94 mmol), ethyl 3-bromo-2,2-dimethylpropanoate (D98) (197 mg, 0.94 mmol) and K2CO3 (130 mg, 0.94 mmol) in DMF (5 ml) was stirred at 80° C. for 48 hours. The reaction mixture was then cooled to room temperature and partitioned between EtOAc and water (30 ml). The organic phase was separated, dried over MgSO4 and concentrated in vacuo. Purification of the residue by flash chromatography on silica gel [20% ethyl acetate/cyclohexane] gave the title compound (100 mg, 22%) as a colourless solid. MS (ES) C24H26ClN5O4 requires 483, found 484 [M+H]+

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to room temperature
  2. custompartitioned between EtOAc and water (30 ml)
  3. customThe organic phase was separated
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customPurification of the residue by flash chromatography on silica gel [20% ethyl acetate/cyclohexane]