HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidin-4-ol → HCID 86682307, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidin-4-ol | HCID 79341 | — |
| Reactant | Methyl 3-oxovalerate | HCID 121699 | — |
| Product | HCID 86682307 | HCID 86682307 | — |
Reaction Steps
59.0 g (583 mmol) of 4-hydroxypiperidine and 79.7 g (612 mmol) of 3-oxovaleric acid methyl ester were heated for 9 h at 110° C., and the resulting methanol was removed via a distillation bridge. The reaction residue was freed from volatiles on a rotary evaporator, taken up in ethanol, and filtered through 600 ml of strongly acidic ion exchanger (Dowex® HCR-W2), concentrated again and purified by column chromatography (silica gel, eluent's gradient from ethyl acetate to ethanol). The pure product fractions were freed from solvent on a rotary evaporator and yielded 63.6 g (55%) of a viscous, clear, colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394324B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-d8ac812f41214e26b1f4b6e4c004b8f2 |
| Source note | uspto-grants-2016_07 |