HRID79281

反应详情

EQUATION

反应方程式

HRID 79281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
82.5 °C

PROCEDURE

实验过程

To a solution of N-(3-ethyl-1-((6-hydroxypyridin-2-yl)methyl)-1H-indazol-4-yl)imidazo[1,2-a]pyridine-3-carboxamide (Example 17, Step A; 50 mg, 0.121 mmol) and 2-(tert-butoxycarbonylamino)ethyl methanesulfonate (71 mg, 0.297 mmol) in N,N-dimethylacetamide (2 mL) was added cesium carbonate (79.0 mg, 0.242 mmol). The mixture was heated to 80-85° C. for 90 minutes. After allowing to cool the mixture was diluted with ethyl acetate and methanol, filtered and concentrated under a stream of nitrogen. The material was purified using preparative thin layer chromatography on silica, eluting with 5% methanol and 1% triethylamine in ethyl acetate to give the product 21.9 mg (33%).

WORKUP

后处理

  1. temperatureto cool the mixture
  2. filtrationfiltered
  3. concentrationconcentrated under a stream of nitrogen
  4. customThe material was purified
  5. washeluting with 5% methanol and 1% triethylamine in ethyl acetate