N-methylpiperazine-1-carboxamide

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: To the solution of piperazine (3 g) in dichloromethane (30 ml) was added methyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was added methyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was added methyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was added methyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was addedmethyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was addedmethyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: Palladium on carbon (300 mg, 10% by wt.) was placed under an inert atmosphere and suspended in EtOH (10 mL). A solution of 4-benzyl-piperazine-1-carboxylic acid methylamide (1.50 g, 6.43 mmol) dissolved in 2:1 v/v EtOH/THF (96 mL) was added. The reaction mixture was placed under H2 atmosphere (1 atmosphere pressure) and stirred overnight. The resulting mixture was filtered through a pad of Celite® and the solvent was concentrated in vacuo to give 916 mg (99%) of the title compound as clear oil. 1H-NMR (300 MHz, DMSO-d6) 6.30 (broad d, 1H), 3.15 to 3.12 (m, 5H), 2.59 to 2.55 (m, 4H), 2.53 (d, 3H). was added The resulting mixture was filtered through a pad of Celite® the solvent was concentrated in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was added methyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was added methyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo

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

実験手順: To the solution of piperazine (3 g) in dichloromethane (30 ml) was addedmethyl isocyanate (2.16 ml) in an ice water bath with stirring. After 10 minutes the mixture was stirred at ambient temperature for 1 hour. The reaction mixture was evaporated in vacuo. The residue was diluted with acetonitrile (15 ml) and crystals were filtered off. The filtrate was evaporated in vacuo. To the residue was added xylene and the solvent was azeotropically removed in vacuo to give N-methyl-1-piperazinecarboxamide (2.43 g) as an oil. After 10 minutes the mixture was stirred at ambient temperature for 1 hour The reaction mixture was evaporated in vacuo The residue was diluted with acetonitrile (15 ml) and crystals were filtered off The filtrate was evaporated in vacuo To the residue was added xylene the solvent was azeotropically removed in vacuo