HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenacyl bromide → (RS)-2-[2-phenyl-2-oxo-ethoxycarbonylmethyl]-piperidine-1-carboxylic tert butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenacyl bromide | HCID 6259 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1-Boc-2-Piperidineacetic Acid | HCID 5058536 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | (RS)-2-[2-phenyl-2-oxo-ethoxycarbonylmethyl]-piperidine-1-carboxylic tert butyl ester | HCID 86629005 | 74.2% |
Reaction Steps
2-Carboxymethyl-piperidine-1-carboxylic acid tert butyl ester (2.86 g) and sodium carbonate (0.62 g) were dissolved in water (30 ml) using gentle warming. A solution of 2-bromoacetophenone (2.33 g) in ethanol (60 ml) was then added and the mixture boiled for 2 h. the mixture was cooled to room temperature and stood for 16 h. The mixture was again boiled for 2 h. solvent removed at reduced pressure and the residue partitioned between water and ethyl acetate. The organic phase was dried (MgSO4) and solvent removed at reduced pressure. The residue was column chromatographed (silica gel, 1:1 ethyl acetate:pentane) to give the title compound (3.14 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07423052B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-b83257f65295424686d7100850becbd2 |
| Source note | uspto-grants-2008_09 |