反应详情

温度

70 °C

One hundred and sixty three g. of N-m-nitrophenyl-2,2-dimethylsuccinimide, as prepared in Example I, was added portion wise at reflux temperature to a mixture of 115 g. of powdered iron, 7 ml. of concentrated HCl, 250 ml. of ethyl alcohol and 200 ml. of water. At completion of addition (approximately one hour), the mixture was allowed to cool to 70° C. and 7 g. of 50% sodium hydroxide was added and the iron oxide was removed by filtration through a Dicalite filter which was washed with several portions of hot ethyl alcohol. Stripping of the filtrate under vacuum yielded 106 g. of a product having a m.p. of 143°-145° C. A portion of the product was recrystallized to a m.p. of 147°-147.5° C. The product was identified as the title compound by analysis of infrared spectra.

1. additionwas added portion wise
2. temperatureat reflux temperature
3. additionto a mixture of 115 g
4. additionAt completion of addition (approximately one hour)
5. customthe iron oxide was removed by filtration through a Dicalite
6. filtrationfilter which
7. washwas washed with several portions of hot ethyl alcohol
8. customStripping of the filtrate under vacuum yielded 106 g
9. customA portion of the product was recrystallized to a m.p. of 147°-147.5° C