反应详情

温度

160 °C

314 g (1.13 mol, 1 eq.) of methyl [3-chloro-5-(trifluoromethyl)-2-pyridinyl]-(cyano)acetate and 22 g (0.38 mol, 0.33 eq.) of sodium chloride are dissolved in a solution of 44 mL of water and 1.1 L of dimethyl sulphoxide. The reaction medium is stirred and heated at 160° C. Once all gas has been given off, the medium is cooled to ambient temperature. 1 L of water and 0.5 L of dichloromethane are added. After separation, the aqueous phase is extracted twice with 0.5 L of dichloromethane. The organic phase is washed twice with 0.5 L of water and dried over magnesium sulphate. After concentration, the crude product is diluted in 100 mL of dichloromethane and eluted with an ethyl acetate/heptane mixture (20/80) on a bed of silica. The filtrate is concentrated so as to produce [3-chloro-5-(trifluoromethyl)-2-pyridinyl]acetonitrile.

1. temperaturethe medium is cooled to ambient temperature
2. customAfter separation
3. extractionthe aqueous phase is extracted twice with 0.5 L of dichloromethane
4. washThe organic phase is washed twice with 0.5 L of water
5. dry with materialdried over magnesium sulphate
6. concentrationAfter concentration
7. additionthe crude product is diluted in 100 mL of dichloromethane
8. washeluted with an ethyl acetate/heptane mixture (20/80) on a bed of silica
9. concentrationThe filtrate is concentrated so as