HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → tert-Butyl 4-(methylcarbamoyl)piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Tert-butyl 4-(chlorocarbonyl)piperazine-1-carboxylate | HCID 11334154 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-Butyl 4-(methylcarbamoyl)piperazine-1-carboxylate | HCID 20768834 | 70% |
Reaction Steps
A solution of 1-Boc-4-(chlorocarbonyl)piperazine (300 mg, 1.22 mmol), pyridine (288.4 mg, 3 equiv), and methylamine (1.83 mmol, 1.5 equiv) in dichloromethane was refluxed overnight. The solution was quenched by the dropwise addition of water. The organic layer was separated, dried over anhydrous Na2SO4, and evaporated in vacuo. The residue was purified by flash chromatography to give the title compound as a solid (˜70% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461339B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-174f1e715bad44828618a05446b48794 |
| Source note | uspto-grants-2013_06 |