Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | (S)-1-Boc-3-methylpiperazine | HCID 7023035 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 29920718 | HCID 29920718 | 100.8% |
Reaction Steps
To a solution of (S)-tert-butyl 3-methylpiperazine-1-carboxylate (50 g, 0.250 mol) in 500 mL of methanol was added formaldehyde (41.6 mL, 0.5 mol, 37% aqueous solution) and formic acid (33 mL, 0.874 mol) and the mixture was heated to 70° C. for 16 hours, then concentrated under reduced pressure. The resulting residue was taken up in EtOAc (500 mL), washed with 10% aqueous potassium carbonate, dried over sodium sulfate and concentrated under reduced pressure to give 54 g (100%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09174981B2 |
|---|
| Source dataset | uspto-grants-2015_11 |
|---|
| ORD ID | ord-0b0a92a2a8874bb49db7985da4dce49c |
|---|
| Source note | uspto-grants-2015_11 |
|---|