Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 2-Methylpiperazine | HCID 66057 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 14090597 | HCID 14090597 | — |
Reaction Steps
2-methylpiperazine (1 g) was dissolved in MeOH (12 ml) and AcOH (1.8 ml) was added. The mixture was cooled down to 0° C., ethyl chloroformate (0.95 ml) was added over 60 min. The mixture was allowed to warm to RT and was stirred overnight. Water was added and MeOH was evaporated off. The residue was extracted with toluene and the org. layers were washed with water. The combined aq. layers were basified to pH 14 with a 2M NaOH solution and extracted with toluene. The combined org. layers were washed with a NaCl solution, dried (Na2SO4) and evaporated off to give 936 mg of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08048881B2 |
|---|
| Source dataset | uspto-grants-2011_11 |
|---|
| ORD ID | ord-309148d102944b4aa0122c4ec5c6d7d4 |
|---|
| Source note | uspto-grants-2011_11 |
|---|