N-(2-phenylpropan-2-yl)acetamide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: Aluminum chloride (41.5 g) was portionwise added to a solution (75 ml) of N-(1-methyl-1-phenylethyl)acetamide (25 g) and acetyl chloride (16.6 g) in dichloroethane under ice-cooling. The mixture was stirred at said temperature for 1 hour and then at 50°-60° C. for 1 hour. After completion of the reaction, the reaction mixture was poured into ice water and extracted with chloroform. The extract was washed with water, dried and concentrated under reduced pressure to give crystals which were then recrystallized from ethyl acetate-isopropyl ether to give 20.4 g of N-(1-(4-acetylphenyl)-1-methylethyl)acetamide. cooling for 1 hour After completion of the reaction extracted with chloroform The extract was washed with water dried concentrated under reduced pressure to give crystals which were then recrystallized from ethyl acetate-isopropyl ether

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

実験手順: Acetyl chloride (62 g) was dropwise added to a solution (1 l) of cumylamine (90 g) and a 48% aqueous solution of sodium hydroxide (70 ml) in toluene under ice-cooling and the mixture was stirred at room temperature for 5 hours. After completion of the reaction, the mixture was neutralized with a saturated aqueous solution of potassium carbonate and extracted with ethyl acetate. The extract was washed with water and dried. The solvent was distilled away under reduced pressure to give 102.3 g of N-(1-methyl-1-phenylethyl)acetamide. After completion of the reaction extracted with ethyl acetate The extract was washed with water dried The solvent was distilled away under reduced pressure

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

実験手順: Acetyl chloride (62 g) was dropwise added to a solution (1 l) of cumylamine (90 g) and a 48% aqueous solution of sodium hydroxide (70 ml) in toluene under ice-cooling and the mixture was stirred at room temperature for 5 hours. After completion of the reaction, the mixture was neutralized with a saturated aqueous solution of potassium carbonate and extracted with ethyl acetate. The extract was washed with water and dried. The solvent was distilled away under reduced pressure to give 102.3 g of N-(1-methyl-1-phenylethyl)acetamide. After completion of the reaction extracted with ethyl acetate The extract was washed with water dried The solvent was distilled away under reduced pressure

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

実験手順: Acetyl chloride (62 g) was dropwise added to a solution (1 l) of cumylamine (90 g) and a 48% aqueous solution of sodium hydroxide (70 ml) in toluene under ice-cooling and the mixture was stirred at room temperature for 5 hours. After completion of the reaction, the mixture was neutralized with a saturated aqueous solution of potassium carbonate and extracted with ethyl acetate. The extract was washed with water and dried. The solvent was distilled away under reduced pressure to give 102.3 g of N-(1-methyl-1-phenylethyl)acetamide. After completion of the reaction extracted with ethyl acetate The extract was washed with water dried The solvent was distilled away under reduced pressure

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

実験手順: A solution of N-(1-methyl-1-phenylethyl)acetamide (21.3 g, 121 mmol), phenylacetyl chloride (19.5 g, 126 mmol) and aluminum trichloride (19 g, 142 mmol) in methylene chloride (140 mL) was stirred overnight at room temperature under an atmosphere of nitrogen. The reaction was poured onto ice and stirred until the ice melted, then the layers were separated and the organic layer was washed with saturated sodium bicarbonate, brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography gave the title compound. MS (M+H+): calculated=295.38, observed=296.1 The reaction was poured onto ice the layers were separated the organic layer was washed with saturated sodium bicarbonate, brine dried over magnesium sulfate filtered concentrated Purification by silica gel chromatography