1-(3-氯苄基)哌嗪-2-酮

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1-(3-chlorobenzyl)piperazin-2-one (3.97 g, 17.67 mmol) and diethyl ethoxymethylenemalonate (4.01 g, 18.55 mmol) in toluene (60 mL) was heated in a sealed tube at 80° C. overnight. The resultant mixture was concentrated under vacuum. The residue was dissolved in anhydrous DMF (200 mL), cooled to 0° C. under an atmosphere of nitrogen, and treated with a solution of lithium bis(trimethylsilyl)amide in THF (1 M, 21.2 mL, 21.2 mmol). The reaction mixture was stirred at room temperature overnight and concentrated under vacuum. The residue was partitioned between ethyl acetate and dilute aqueous HCl. The organic extract was washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was triturated with diethyl ether, and the solid precipitated was filtered to provide the title compound. The resultant mixture was concentrated under vacuum The residue was dissolved in anhydrous DMF (200 mL) cooled to 0° C. under an atmosphere of nitrogen concentrated under vacuum The residue was partitioned between ethyl acetate and dilute aqueous HCl The organic extract was washed with brine dried over anhydrous magnesium sulfate filtered concentrated under vacuum The residue was triturated with diethyl ether the solid precipitated was filtered

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1-(3-chlorobenzyl)piperazin-2-one (3.97 g, 17.67 mmol) and diethyl ethoxymethylenemalonate (4.01 g, 18.55 mmol) in toluene (60 mL) was heated in a sealed tube at 80° C. overnight. The resultant mixture was concentrated under vacuum. The residue was dissolved in anhydrous DMF (200 mL), cooled to 0° C. under an atmosphere of nitrogen, and treated with a solution of lithium bis(trimethylsilyl)amide in THF (1 M, 21.2 mL, 21.2 mmol). The reaction mixture was stirred at room temperature overnight and concentrated under vacuum. The residue was partitioned between ethyl acetate and dilute aqueous HCl. The organic extract was washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was triturated with diethyl ether, and the solid precipitated was filtered to provide the title compound. The resultant mixture was concentrated under vacuum The residue was dissolved in anhydrous DMF (200 mL) cooled to 0° C. under an atmosphere of nitrogen concentrated under vacuum The residue was partitioned between ethyl acetate and dilute aqueous HCl The organic extract was washed with brine dried over anhydrous magnesium sulfate filtered concentrated under vacuum The residue was triturated with diethyl ether the solid precipitated was filtered