反应详情

温度

0 °C

To a mixture of 4-chloro-5-fluoro-nicotinonitrile (1.0 g, 6.4 mmol) and potassium carbonate (4.4 g, 32 mmol) in DMF (15 mL) at 0° C. was added ethyl thioglycolate (0.73 mL, 6.7 mmol) dropwise. The reaction mixture was stirred at 0° C. for 10 min, at room temperature for 20 min and then at 40° C. for 30 min. The reaction mixture was cooled to room temperature and partitioned between water and ethyl acetate. The organic layer was separated and washed with water followed by brine, dried over sodium sulphate and concentrated in vacuo to give the title compound as a yellow solid (1.5 g, quant.). LCMS (method B): RT=3.41 min, M+H+=241.

1. waitat 40° C. for 30 min
2. temperatureThe reaction mixture was cooled to room temperature
3. custompartitioned between water and ethyl acetate
4. customThe organic layer was separated
5. washwashed with water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated in vacuo