Piperazine → N-methylpiperazine-1-carboxamide

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.

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-e5cd8b0616c34d2792fa9978d79ed01d

Source dataset

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05922711