反应详情

温度

60 °C

A mixture of 19.5 g (0.075 mole) of N-(2-(2,4-dichlorophenoxy)ethyl)propylamide, 11.4 g (0.075 mole) POCl3 and 250 mls of 1,2-dichloroethane was stirred at 60° C. for six hours. The mixture was cooled to 25° C., whereupon 10.4 g (0.075 mole) of 4-chloro-2-methylaniline was added thereto. An exotherm was noted. The mixture was refluxed for 10 hours and allowed to cool. The product mixture was made basic with a 20% NaOH water solution. The product layer was separated, washed once with 200 ml of water, dried over sodium sulfate, filtered and distilled under reduced pressure to give 65% yield (based on the amide) of the desired product, a thick oil, b.p. 142° C./1.3 mm Hg . NMR confirmed the assigned structure: ##STR4##

1. additionwas added
2. temperatureThe mixture was refluxed for 10 hours
3. temperatureto cool
4. customThe product layer was separated
5. washwashed once with 200 ml of water
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. distillationdistilled under reduced pressure
9. customto give 65% yield (