2-[2-(2,6-二氯苯胺)苯基]-N,N-二甲基乙酰胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 40 ml of a 15% ethanol solution of potassium hydroxide was added 1.7 g of N,N-dimethyl-o-(2,6-dichloroanilino)phenylacetamide, and the mixture was agitated under reflux for 4 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and 30 ml of water was added to the residue and the mixture was made acidic by hydrochloric acid at a temperature lower than 5° C. The precipitated crystal was recovered by filtration under suction, washed with water and dried. Recrystallization from a mixed solvent of ether and petroleum ether gave 1.45 g of a colorless crystal having a melting point of 158° to 160° C. The yield was 92.9%. under reflux for 4 hours After completion of the reaction the solvent was removed by distillation under reduced pressure, and 30 ml of water was added to the residue was made acidic by hydrochloric acid at a temperature lower than 5° C The precipitated crystal was recovered by filtration under suction washed with water dried Recrystallization from a mixed solvent of ether and petroleum ether

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 40 ml of a 15% ethanol solution of potassium hydroxide was added 1.7 g of N,N-dimethyl-o-(2,6-dichloroanilino)phenylacetamide, and the mixture was agitated under reflux for 4 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and 30 ml of water was added to the residue and the mixture was made acidic by hydrochloric acid at a temperature lower than 5° C. The precipitated crystal was recovered by filtration under suction, washed with water and dried. Recrystallization from a mixed solvent of ether and petroleum ether gave 1.45 g of a colorless crystal having a melting point of 158° to 160° C. The yield was 92.9%. under reflux for 4 hours After completion of the reaction the solvent was removed by distillation under reduced pressure, and 30 ml of water was added to the residue was made acidic by hydrochloric acid at a temperature lower than 5° C The precipitated crystal was recovered by filtration under suction washed with water dried Recrystallization from a mixed solvent of ether and petroleum ether

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In 80 ml of xylene (having a boiling point of 138° to 141° C.), 8.5 g (0.0525 mole) of 2,6-dichloroaniline was refluxed together with 5.2 g (0.0215 mole) of N,N-dimethyl-o-bromophenylacetamide, 5.0 g (0.0357 mole) of potassium carbonate, 1.0 g of copper powder, 1.0 g of cuprous iodide and 2.0 g of sodium iodide for 48 hours under agitation, while water formed by the reaction was being separated. After completion of the reaction, the reaction mixture was treated with active carbon while it was still warm, and the filtrate was concentrated. The obtained residue was mixed with methyl alcohol and the crystal precipitated on cooling was recovered by filtration, washed with methyl alcohol and dried. formed by the reaction was being separated After completion of the reaction the reaction mixture was treated with active carbon while it was still warm the filtrate was concentrated The obtained residue was mixed with methyl alcohol the crystal precipitated on cooling was recovered by filtration washed with methyl alcohol dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 40 ml of a 15% ethanol solution of potassium hydroxide was added 1.7 g of N,N-dimethyl-o-(2,6-dichloroanilino)phenylacetamide, and the mixture was agitated under reflux for 4 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and 30 ml of water was added to the residue and the mixture was made acidic by hydrochloric acid at a temperature lower than 5° C. The precipitated crystal was recovered by filtration under suction, washed with water and dried. Recrystallization from a mixed solvent of ether and petroleum ether gave 1.45 g of a colorless crystal having a melting point of 158° to 160° C. The yield was 92.9%. under reflux for 4 hours After completion of the reaction the solvent was removed by distillation under reduced pressure, and 30 ml of water was added to the residue was made acidic by hydrochloric acid at a temperature lower than 5° C The precipitated crystal was recovered by filtration under suction washed with water dried Recrystallization from a mixed solvent of ether and petroleum ether

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In 80 ml of xylene (having a boiling point of 138° to 141° C.), 8.5 g (0.0525 mole) of 2,6-dichloroaniline was refluxed together with 5.2 g (0.0215 mole) of N,N-dimethyl-o-bromophenylacetamide, 5.0 g (0.0357 mole) of potassium carbonate, 1.0 g of copper powder, 1.0 g of cuprous iodide and 2.0 g of sodium iodide for 48 hours under agitation, while water formed by the reaction was being separated. After completion of the reaction, the reaction mixture was treated with active carbon while it was still warm, and the filtrate was concentrated. The obtained residue was mixed with methyl alcohol and the crystal precipitated on cooling was recovered by filtration, washed with methyl alcohol and dried. formed by the reaction was being separated After completion of the reaction the reaction mixture was treated with active carbon while it was still warm the filtrate was concentrated The obtained residue was mixed with methyl alcohol the crystal precipitated on cooling was recovered by filtration washed with methyl alcohol dried