HRID659960

反应详情

EQUATION

反应方程式

HRID 659960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

560 mg (1.66 mmoles) of 3-(4-Fluoro-phenyl)-2-(2-methylthio-pyrimidin-4-yl)-1H-pyrrolo[3,2-b]pyridine is stirred at room temperature in a mixture of 50 mL of absolute ethanol and 40 mL of ammonia (15% in water). 2 g of Raney nickel (50% in water) is then added to the solution which is further stirred for 3 hours under refluxing conditions. Once cooled, the reaction mixture is filtered over celite and extracted with ethyl acetate. The organic phase is washed with water and dried over magnesium sulfate. The solid residue after concentration is solubilised in ethyl acetate and purified by chromatography on silica gel (ethylacetate/hexane 1/1) to give 250 mg of 3-(4-Fluoro-phenyl)-2-pyrimidin-4-yl-1H-pyrrolo[3,2-b]pyridine as yellowish solid.

WORKUP

后处理

  1. temperatureOnce cooled
  2. filtrationthe reaction mixture is filtered over celite
  3. extractionextracted with ethyl acetate
  4. washThe organic phase is washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe solid residue after concentration
  7. custompurified by chromatography on silica gel (ethylacetate/hexane 1/1)