HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1,3-Dimethyl 2-(4-((tert-butoxy)carbonyl)piperazin-1-yl)propanedioate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Dimethyl bromomalonate | HCID 70087 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1,3-Dimethyl 2-(4-((tert-butoxy)carbonyl)piperazin-1-yl)propanedioate | HCID 57848692 | 97% |
Reaction Steps
19.5 g (141 mmol) of potassium carbonate then 19.5 ml (134 mmol) of dimethyl bromomalonate are added to a solution of 25 g (134 mmol) of tert-butyl piperazine-1-carboxylate in 300 ml of acetonitrile. The reaction medium is stirred at ambient temperature for 24 h then filtered to remove the insoluble salts and concentrated under vacuum. The crude residue obtained is purified by chromatography by silica gel eluted with a 70/30 heptane/ethyl acetate mixture. 41 g (97%) of dimethyl 2-(4-tert-butoxycarbonylpiperazin-1-yl)malonate are obtained in the form of a clear oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115102B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-f2591c8401144a44ae7ed4ac1eacd7db |
| Source note | uspto-grants-2015_08 |