反应详情

A solution of bromine (10.9 mL, 33.6 g, 0.21 mol) in carbon tetrachloride is added to a mixture of p-chloro-β-(methylamino)cinnamonitrile, (E)- or (Z)- (38.53 g, 0.2 mol) in carbon tetrachloride and tetrahydrofuran at 55°-60° C. over 30 minutes. The reaction mixture is cooled to room temperature, concentrated in vacuo to one-half of the original volume and filtered to obtain a solid. The solid is diluted with carbon tetrachloride and the resulting mixture is heated at reflux, cooled and filtered to give the title product as a yellow solid (43.6 g, mp 178°-178.5° C.) which is identified by 1H and 13CNMR spectral analyses.

1. concentrationconcentrated in vacuo to one-half of the original volume
2. filtrationfiltered
3. customto obtain a solid
4. temperaturethe resulting mixture is heated
5. temperatureat reflux
6. temperaturecooled
7. filtrationfiltered