Piperazine → N-methylpiperazine-1-carboxamide

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.

1. stirringAfter 10 minutes the mixture was stirred at ambient temperature for 1 hour
2. customThe reaction mixture was evaporated in vacuo
3. additionThe residue was diluted with acetonitrile (15 ml) and crystals
4. filtrationwere filtered off
5. customThe filtrate was evaporated in vacuo
6. additionTo the residue was added xylene
7. customthe solvent was azeotropically removed in vacuo

ORD record

ord-747e3db665564ee7999c7b06f35448ae

Source dataset

uspto-grants-1996_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05563162