反应详情

A mixture of N-{[2,3-dichloro-4-cyano-5-(3,4-dichlorophenyl)pyrrol-1-yl]methyl}acetamide (3.2 g, 0.0085 mol) and phosphorus oxychloride (6.51 g, 4 mL, 0.0424 mol) is heated at reflux temperature for 40 minutes, cooled, diluted with water and extracted with ethyl acetate. The combined organic extracts are washed sequentially with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a solid. Recrystallization of the solid from an ethyl acetate/heptane solution gives the title product as a pale brown solid (2.35 g, mp 153°-156.0° C.) which is identified by IR and NMR spectral analyses.

1. temperatureis heated
2. temperatureat reflux temperature for 40 minutes
3. temperaturecooled
4. extractionextracted with ethyl acetate
5. washThe combined organic extracts are washed sequentially with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. customto obtain a solid
9. customRecrystallization of the solid from an ethyl acetate/heptane solution