反应详情

温度

90 °C

To a solution of 25 g 2-(4-chloro-phenyl)-3-cyclopropylmethoxy-pyridine 1-oxide in 500 mL acetonitrile, 9.23 g triethylamine and 10.73 g dimethylcarbamoylchlorid were added. After 5 minutes at room temperature, 27.88 g trimethylsilylcyanid was added. The reaction mixture was stirred at 90° C. over 15 h. The reaction mixture was partitioned between water and ethyl acetate; then extracted. The organic phase was washed with brine; then dried over MgSO4 and purified by chromatography on silica gel with a gradient of heptane to heptane:ethyl acetate 2:1 to yield 15.30 g (59.26%) of the title compound as light yellow solid, MS 285.1 (M+H)+.

1. customThe reaction mixture was partitioned between water and ethyl acetate
2. extractionthen extracted
3. washThe organic phase was washed with brine
4. dry with materialthen dried over MgSO4
5. custompurified by chromatography on silica gel with a gradient of heptane to heptane:ethyl acetate 2:1