HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Piperidone hydrochloride → tert-Butyl 4-oxopiperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Piperidone hydrochloride | HCID 3084851 | — |
| Reactant | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
Reaction Steps
4-Ketopiperidine hydrochloride (48.3 g) and di-tert-butyl carbonate (93.2 g) were dissolved in a dioxane-water equivolume mixture (1000 ml), and triethylamine (119 ml) was added to the resultant mixture. The mixture was stirred at room temperature for five hours and concentrated under reduced pressure. Water and ethyl acetate were added to the residue. After separation of the organic phase, the organic phase was washed with a saturated solution of potassium hydrogensulfate and water, dried over sodium sulfate anhydrate, and concentrated under reduced pressure, to thereby obtain the title compound as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06107308 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-d4e61fced110421d873f0cab193649c4 |
| Source note | uspto-grants-2000_08 |