反应详情

温度

70 °C

A solution of p-chloro-β-(methylamino)cinnamonitrile (19.3 g, 0.1 mol) in carbon tetrachloride at 70° C. is treated dropwise with a solution of bromine (16.8 g, 0.105 mol) in carbon tetrachloride over a 30-40 minute period (tetrahydrofuran is added as needed during the bromine addition to aid dissolution of the reaction mixture). The reaction mixture is stirred for 30 minutes at 70° C., cooled to room temperature and concentrated to give a yellow crystalline precipitate. The mixture is filtered, the filter cake is washed with carbon tetrachloride and dried to give the title product as a yellow solid, 18.8 g (69% yield), mp 178.0°-178.5° C., identified by IR, NMR and mass spectral analyses.

1. additionis added
2. dissolutiondissolution of the reaction mixture)
3. temperaturecooled to room temperature
4. concentrationconcentrated
5. customto give a yellow crystalline precipitate
6. filtrationThe mixture is filtered
7. washthe filter cake is washed with carbon tetrachloride
8. customdried