反应详情

5-Fluoro-4-methylamino-nicotinonitrile (2.35 g, 15 mmol) was dissolved in DMF (50 mL) and the solution cooled in an ice-bath. This solution was treated portionwise with sodium hydride (900 mg, 60% in oil, 22.5 mmol). The mixture was allowed to warm to room temperature and stirring continued for 15 minutes at room temperature. Ethyl bromoacetate (2.49 ml, 22.5 mmol) was added and the mixture stirred for 30 minutes at room temperature The reaction mixture was quenched with water and extracted with ethyl acetate. The organic layer was isolated, dried (Na2SO4) and evaporated to give a solid. Trituration of the resultant solid with methanol gave the title compound (1.85 g, 52%) as a yellow solid. LCMS (method B): RT=2.09 min, M+H+ 238.

1. temperaturethe solution cooled in an ice-bath
2. stirringthe mixture stirred for 30 minutes at room temperature The reaction mixture
3. customwas quenched with water
4. extractionextracted with ethyl acetate
5. customThe organic layer was isolated
6. dry with materialdried (Na2SO4)
7. customevaporated
8. customto give a solid