反应详情

温度

100 °C

A mixture of 4-hydroxy-5-iodonicotinonitrile (57.5 g, 234 mmol) and POCl3 (200 mL) was heated at 100° C. for 2 hours, cooled to room temperature and evaporated to remove excess POCl3. The residue was cooled in an ice-water bath, adjusted to pH 8-9 with aqueous 10 N NaOH and extracted with ethyl acetate. The combined organics were washed with water and brine, dried over magnesium sulfate and concentrated. The resulting solid residue was washed with a minimum amount of methanol and methylene chloride to give 46.5 g (75%) of 4-chloro-5-iodonicotinonitrile as a tan solid. Melting range: 120-122° C.

1. temperaturecooled to room temperature
2. customevaporated
3. customto remove excess POCl3
4. temperatureThe residue was cooled in an ice-water bath
5. extractionextracted with ethyl acetate
6. washThe combined organics were washed with water and brine
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated
9. washThe resulting solid residue was washed with a minimum amount of methanol and methylene chloride