HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-Dimethylethyl 4-[(1E)-4-(dimethoxyphosphinyl)-3-oxo-1-buten-1-yl]-1-piperidinecarboxylate → HCID 21993678, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-Dimethylethyl 4-[(1E)-4-(dimethoxyphosphinyl)-3-oxo-1-buten-1-yl]-1-piperidinecarboxylate | HCID 131722578 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 21993678 | HCID 21993678 | — |
Reaction Steps
A solution of 5.443 g (15.062 mM) of tert-butyl (E)-4-[4-(dimethoxyphosphoryl)-3-oxo-1-butenyl]piperidine-1-carboxylate in 50 ml of methanol was subjected to hydrogenation using 3 g of 10% palladium-on-carbon (50% hydrous) as a catalyst at room temperature and atmospheric pressure until the starting material had been no longer detected. The catalyst was removed by filtration with the aid of celite and the catalyst was washed with methanol. The filtrate and washes were pooled and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate:1/1 to ethyl acetate) to provide the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06235731B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-68d15202cf8b4550b80bd92b7b03beb8 |
| Source note | uspto-grants-2001_05 |