1-(4-氯丁基)-4-甲基哌嗪

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

实验步骤: In a 2 L three-necked round bottomed flask was added N-methyl-piperazine (100.16 g, 1.0 mol), acetone (1000 mL), and anhydrous potassium carbonate (276.42 g, 2.0 mol, 2.0 equiv.). The flask was equipped with a mechanical stirrer and a condenser. 4-chloro-1-bromo-butane (188.6 g, 1.1 mol, 1.1 equiv.) was added dropwise under continuous stirring at room temperature over a period of 30 min. The suspension mixture was then stirred at 40° C. The progress of the reaction was monitored by TLC, which confirmed the reaction was completed after 4 hours. The mixture was cooled to room temperature and the insoluble materials were removed by filtration and washed with dichloromethane (2×100 mL). The combined filtrates were concentrated under vacuum until they became dry. The residue was then mixed with dichloromethane (500 mL). Insoluble materials were removed by filtration and washed by dichloromethane (2×100 mL). The combined filtrate and washings were concentrated and purified through a flash silica gel column, which gave the expected product as light yellow oil. (92.5 g, 48.5% yield). The flask was equipped with a mechanical stirrer and a condenser The suspension mixture was then stirred at 40° C was completed after 4 hours The mixture was cooled to room temperature the insoluble materials were removed by filtration washed with dichloromethane (2×100 mL) The combined filtrates were concentrated under vacuum until they became dry The residue was then mixed with dichloromethane (500 mL) Insoluble materials were removed by filtration washed by dichloromethane (2×100 mL) The combined filtrate and washings were concentrated purified through a flash silica gel column, which

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

实验步骤: In a 2 L three-necked round bottomed flask was added N-methyl-piperazine (100.16 g, 1.0 mol), acetone (1000 mL), and anhydrous potassium carbonate (276.42 g, 2.0 mol, 2.0 equiv.). The flask was equipped with a mechanical stirrer and a condenser. 4-chloro-1-bromo-butane (188.6 g, 1.1 mol, 1.1 equiv.) was added dropwise under continuous stirring at room temperature over a period of 30 min. The suspension mixture was then stirred at 40° C. The progress of the reaction was monitored by TLC, which confirmed the reaction was completed after 4 hours. The mixture was cooled to room temperature and the insoluble materials were removed by filtration and washed with dichloromethane (2×100 mL). The combined filtrates were concentrated under vacuum until they became dry. The residue was then mixed with dichloromethane (500 mL). Insoluble materials were removed by filtration and washed by dichloromethane (2×100 mL). The combined filtrate and washings were concentrated and purified through a flash silica gel column, which gave the expected product as light yellow oil. (92.5 g, 48.5% yield). The flask was equipped with a mechanical stirrer and a condenser The suspension mixture was then stirred at 40° C was completed after 4 hours The mixture was cooled to room temperature the insoluble materials were removed by filtration washed with dichloromethane (2×100 mL) The combined filtrates were concentrated under vacuum until they became dry The residue was then mixed with dichloromethane (500 mL) Insoluble materials were removed by filtration washed by dichloromethane (2×100 mL) The combined filtrate and washings were concentrated purified through a flash silica gel column, which