HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Acetate → HCID 22727172, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 4-Chloro-2-methylpyridine | HCID 581392 | — |
| Reactant | Piperidone monohydrate hydrochloride | HCID 22021827 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 22727172 | HCID 22727172 | 83.1% |
Reaction Steps
A mixture of piperidone hydrochloride hydrate (68.98 g), 4-chloro-2-picolin (47.7 g) and sodium acetate (36.8 g) in acetic acid (500 ml) was refluxed for 15 hours and then the reaction mixture was concentrated, and the resultant residue was dissolved in water, combined with potassium hydroxide to make alkaline, and then extracted with dichloromethane, dried and concentrated. The residue obtained was purified by a column chromatography on a silica gel (dichloromethane: 10% aqueous ammonia-containing methanol=30:1) to obtain the title compound (59.1 g) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06723722B1 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-294b873d65a84cbf92946f4a98cf0f7f |
| Source note | uspto-grants-2004_04 |