N-(2,5-dichlorophenyl)acetamide

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 2.5 liter flask is charged with 550 g of petroleum distillate (boiling range: 110°-140° C.). With stirring, 162.0 g of 100% 2,5-dichloroaniline are then added and the mixture is warmed to 45° C., whereupon a solution forms. The 108 g of 100% acetic anhydride are added dropwise in the course of about 15 minutes and the temperature is allowed to rise to 65° C. After the reaction mixture has been stirred for 15 minutes at 65° C., the addition of 1265 g of 98% sulfuric acid is commenced, while ensuring that the temperature does not rise substantially above 70°-75° C. After addition of about 20-25% of the sulfuric acid, the precipitated acetanilide starts to dissolve. Hardly any further exothermic reaction ensues when the remainder of the sulfuric acid is added, and the temperature falls to about 60° C. The temperature of the 2-phase mixture is brought to 20°-25° C. by further cooling, and the feed of 128.2 g of 50.2% nitrating acid is commenced immediately at a temperature not higher than 25° C. The addition is complete after about 50 minutes and the reaction mixture is stirred for a further 20 minutes at 20° to 25° C. to rise to 65° C After the reaction mixture has been stirred for 15 minutes at 65° C. does not rise substantially above 70°-75° C to dissolve Hardly any further exothermic reaction is added falls to about 60° C is brought to 20°-25° C. by further cooling is commenced immediately at a temperature not higher than 25° C The addition the reaction mixture is stirred for a further 20 minutes at 20° to 25° C.