HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 58285194, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Chloro-4-(chloromethyl)pyridine | HCID 11126573 | — |
| Reactant | tert-Butyl 4-(methylcarbamoyl)piperazine-1-carboxylate | HCID 20768834 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58285194 | HCID 58285194 | 90% |
Reaction Steps
1-Boc-4-(N-methylcarbamoyl)piperazine was treated with 8 M HCl/EtOAc to afford a salt, then the salt (1.0 equiv) was mixed with 2-chloro-4-(chloromethyl)pyridine (1.0 equiv) (Preparation B-11) and K2CO3 (4 equiv) in DMF. The mixture was stirred for 1 h at rt. After removing most of the solvent, the residue was partitioned in water and EtOAc. 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 (˜90% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461339B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-421de3c6519448129cf2e9abaa89b343 |
| Source note | uspto-grants-2013_06 |