3,3-dimethylpiperazin-2-one

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:

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:

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: Potassium carbonate (390 grams) and ethylene diamine (1001 grams) are stirred with toluene (1.50 l). A solution of ethyl 2-bromoisobutyrate (500 grams) in toluene (750 ml) is added. The suspension is heated to reflux over night, and filtered. The filter cake is washed with toluene (500 ml). The combined filtrates (volume 4.0 l) are heated on a water bath and distilled at 0.3 atm. using a Claisen apparatus; first 1200 ml distillate is collected at 35° C. (the temperature in the mixture is 75° C.). More toluene is added (600 ml), and another 1200 ml distillate is collected at 76° C. (the temperature in the mixture is 80° C.). Toluene (750 ml) is added again, and 1100 ml of distillate is collected at 66° C. (temperature in the mixture 71° C.). The mixture is stirred on an ice bath and seeded, whereby the product precipitates. The product is isolated by filtration, washed with toluene, and dried over night in a vacuum oven at 50° C. Yield 171 g (52%) of 3,3-dimethylpiperazin-2-one. NMR consistent with structure. The suspension is heated to reflux over night filtered The filter cake is washed with toluene (500 ml) The combined filtrates (volume 4.0 l) are heated on a water bath distilled at 0.3 atm. first 1200 ml distillate is collected at 35° C. (the temperature in the mixture is 75° C. More toluene is added (600 ml) another 1200 ml distillate is collected at 76° C. (the temperature in the mixture is 80° C. Toluene (750 ml) is added again 1100 ml of distillate is collected at 66° C. (temperature in the mixture 71° C.) whereby the product precipitates The product is isolated by filtration washed with toluene dried over night in a vacuum oven at 50° C

反応条件: temp:42.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3,3-dimethylpiperazin-2-one (50 grams) is suspended in 1,2-dimethoxyethane (DME) (150 ml) and potassium carbonate (70 grams) is added. Methyl iodide (66.4 grams) is added during half an hour, while the mixture is cooled slightly, allowing the temperature to reach 50° C. The mixture is stirred 9 hours at an oil bath at 40-45° C., and a sample is withdrawn for NMR, which indicates, that there is still 8% starting material left (singal at 2.8 ppm). More methyl iodide is added (4.6 grams), and the mixture is stirred for another 2½ hour at 40° C., and a new NMR sample shows full conversion. The mixture is filtered, and the filter cake is washed with DME. The filtrate is evaporated to dryness giving 41 grams of the title compound. NMR complies with the structure. is cooled slightly to reach 50° C a sample is withdrawn for NMR, which left (singal at 2.8 ppm) More methyl iodide is added (4.6 grams) the mixture is stirred for another 2½ hour at 40° C. The mixture is filtered the filter cake is washed with DME The filtrate is evaporated to dryness

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

実験手順: Potassium carbonate (390 grams) and ethylene diamine (1001 grams) are stirred with toluene (1.50 l). A solution of ethyl 2-bromoisobutyrate (500 grams) in toluene (750 ml) is added. The suspension is heated to reflux over night, and filtered. The filter cake is washed with toluene (500 ml). The combined filtrates (volume 4.01) are heated on a water bath and distilled at 0.3 atm. using a Claisen apparatus; first 1200 ml distillate is collected at 35° C. (the temperature in the mixture is 75° C.). More toluene is added (600 ml), and another 1200 ml distillate is collected at 76° C. (the temperature in the mixture is 80° C.). Toluene (750 ml) is added again, and 1100 ml of distillate is collected at 66° C. (temperature in the mixture 71° C.). The mixture is stirred on an ice bath and inoculated, whereby the product precipitates. The product is isolated by filtration, washed with toluene, and dried over night in a vacuum oven at 50° C. Yield 171 g (52%) of 3,3-dimethylpiperazin-2-one. NMR consistent with structure. The suspension is heated to reflux over night filtered The filter cake is washed with toluene (500 ml) The combined filtrates (volume 4.01) are heated on a water bath distilled at 0.3 atm. first 1200 ml distillate is collected at 35° C. (the temperature in the mixture is 75° C. More toluene is added (600 ml) another 1200 ml distillate is collected at 76° C. (the temperature in the mixture is 80° C. Toluene (750 ml) is added again 1100 ml of distillate is collected at 66° C. (temperature in the mixture 71° C.) whereby the product precipitates The product is isolated by filtration washed with toluene dried over night in a vacuum oven at 50° C

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

実験手順: Potassium carbonate (390 grams) and ethylene diamine (1001 grams) are stirred with toluene (1.50 l). A solution of ethyl 2-bromoisobutyrate (500 grams) in toluene (750 ml) is added. The suspension is heated to reflux over night, and filtered. The filter cake is washed with toluene (500 ml). The combined filtrates (volume 4.01) are heated on a water bath and distilled at 0.3 atm. using a Claisen apparatus; first 1200 ml distillate is collected at 35° C. (the temperature in the mixture is 75° C.). More toluene is added (600 ml), and another 1200 ml distillate is collected at 76° C. (the temperature in the mixture is 80° C.). Toluene (750 ml) is added again, and 1100 ml of distillate is collected at 66° C. (temperature in the mixture 71° C.). The mixture is stirred on an ice bath and inoculated, whereby the product precipitates. The product is isolated by filtration, washed with toluene, and dried over night in a vacuum oven at 50° C. Yield 171 g (52%) of 3,3-dimethylpiperazin-2-one. NMR consistent with structure. The suspension is heated to reflux over night filtered The filter cake is washed with toluene (500 ml) The combined filtrates (volume 4.01) are heated on a water bath distilled at 0.3 atm. first 1200 ml distillate is collected at 35° C. (the temperature in the mixture is 75° C. More toluene is added (600 ml) another 1200 ml distillate is collected at 76° C. (the temperature in the mixture is 80° C. Toluene (750 ml) is added again 1100 ml of distillate is collected at 66° C. (temperature in the mixture 71° C.) whereby the product precipitates The product is isolated by filtration washed with toluene dried over night in a vacuum oven at 50° C