N1-(2-氯苯基)-2-氯乙酰胺

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

实验步骤: The product of step (i) (5.9 g) was dissolved in ethanol (50 ml) and cis-2,6-dimethylpiperazine (3 g) and sodium hydrogencarbonate (6.63 g) were added at room temperature under a nitrogen atmosphere. The mixture was heated under reflux for 24 hours and the cooled solution was filtered and the filtrate was evaporated under reduced pressure. The residue was dissolved in 1M HCl (22 ml) and washed with dichloromethane. The aqueous solution was then basified to pH13 with a solution of sodium hydroxide and the product was extracted with dichloromethane. The organic layer was washed with water, brine, collected, dried (MgSO4) and concentrated under reduced pressure to give the subtitle compound as a beige solid. Yield 4 g. The mixture was heated under reflux for 24 hours the cooled solution was filtered the filtrate was evaporated under reduced pressure The residue was dissolved in 1M HCl (22 ml) washed with dichloromethane the product was extracted with dichloromethane The organic layer was washed with water, brine collected dried (MgSO4) concentrated under reduced pressure

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroaniline (5 g) was dissolved in dichloromethane (100 ml) and chloroacetyl chloride (3.11 ml) and N,N-diisopropylethylamine (13.65 ml) were added at 0° C. under a nitrogen atmosphere. The mixture was stirred for 1 hour at 0° C. and 12 hours at room temperature, then quenched with water. The product was extracted with dichloromethane. The organic layer was washed with water, brine, dried (MgSO4) and concentrated under reduced pressure to leave the subtitle product as a beige solid. Yield 7.5 g. This was used in the next step without further purification. quenched with water The product was extracted with dichloromethane The organic layer was washed with water, brine dried (MgSO4) concentrated under reduced pressure

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

实验步骤: The product of step (i) (5.9 g) was dissolved in ethanol (50 ml) and cis-2,6-dimethylpiperazine (3 g) and sodium hydrogencarbonate (6.63 g) were added at room temperature under a nitrogen atmosphere. The mixture was heated under reflux for 24 hours and the cooled solution was filtered and the filtrate was evaporated under reduced pressure. The residue was dissolved in 1M HCl (22 ml) and washed with dichloromethane. The aqueous solution was then basified to pH13 with a solution of sodium hydroxide and the product was extracted with dichloromethane. The organic layer was washed with water, brine, collected, dried (MgSO4) and concentrated under reduced pressure to give the subtitle compound as a beige solid. Yield 4 g. The mixture was heated under reflux for 24 hours the cooled solution was filtered the filtrate was evaporated under reduced pressure The residue was dissolved in 1M HCl (22 ml) washed with dichloromethane the product was extracted with dichloromethane The organic layer was washed with water, brine collected dried (MgSO4) concentrated under reduced pressure

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroaniline (5 g) was dissolved in dichloromethane (100 ml) and chloroacetyl chloride (3.11 ml) and N,N-diisopropylethylamine (13.65 ml) were added at 0° C. under a nitrogen atmosphere. The mixture was stirred for 1 hour at 0° C. and 12 hours at room temperature, then quenched with water. The product was extracted with dichloromethane. The organic layer was washed with water, brine, dried (MgSO4) and concentrated under reduced pressure to leave the subtitle product as a beige solid. Yield 7.5 g. This was used in the next step without further purification. quenched with water The product was extracted with dichloromethane The organic layer was washed with water, brine dried (MgSO4) concentrated under reduced pressure