HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(4-Methyl-piperazine-1-carbonyl)-piperidin-4-one hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Methylpiperazine-1-carbonyl chloride monohydrochloride | HCID 3016934 | — |
| Reactant | Piperidone monohydrate hydrochloride | HCID 22021827 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(4-Methyl-piperazine-1-carbonyl)-piperidin-4-one hydrochloride | HCID 57444160 | 50% |
Reaction Steps
To a suspension of 4-methylpiperazine-1-carbonyl chloride hydrochloride (19.9 g 0.1 mol) and piperidone monohydrate hydrochloride (15.3 g 0.1 mol), in 200 mL of dichloromethane, dry triethylamine (45 mL, 0.33 mol) was added dropwise. The mixture was stirred for 2 hours. The organic phase was washed with brine (2×20 mL) and dried over sodium sulfate. After filtration, the solvent was evaporated in vacuo and the crude product was dissolved in EtOH (50 mL) and diethylether (100 mL) and treated with HCl 4N in dioxane (25 mL). After 1 hour, the precipitate was filtered and dried in oven to give 13 g (yield 50%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08541429B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-64ff0a64e8ce4469a9ff38d93ccfe498 |
| Source note | uspto-grants-2013_09 |