HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 21183785, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | 1-(Diphenylmethyl)azetidin-3-yl methanesulfonate | HCID 2758716 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21183785 | HCID 21183785 | 87.7% |
Reaction Steps
A mixture of N-tert-butoxycarbonylpiperazine (14.08 g), potassium carbonate (26.1 g), and 1-diphenylmethyl-3-methanesulphonyloxyazetidine (WO 96/05193) (20 g) in dry acetonitrile (600 mL) was heated under reflux for 32 hours. The reaction mixture was cooled to room temperature, diluted with ethyl acetate and washed with water and brine. The organic phase was dried over sodium sulphate and evaporated to dryness in vacuo. The residue was purified by column chromatography over silica (dichloromethane/methanol 97/3 by volume) to afford the title compound as a solid (22.53 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06262046B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-ccafc8a53a42491bb15ec11e08d15693 |
| Source note | uspto-grants-2001_07 |