HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 59264606, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 2-bromo-2-methylpropionate | HCID 90097 | — |
| Reactant | Piperonylamine | HCID 2723901 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 59264606 | HCID 59264606 | — |
Reaction Steps
A mixture of methyl 2-bromo-2-methylpropanoate (80.87 ml, 5 equiv), 4-piperidone hydrochloride monohydrate (19.6 g, 1 equiv), acetonitrile (200 ml) and potassium carbonate (69.1 g, 4 equiv) was heated at reflux under nitrogen with mechanical stirring for 17.5 h then cooled in an ice bath before adding diethyl ether (100 ml). Filtration through celite followed by flash chromatography (silica, 10-50% ethyl acetate in hexane) and evaporation of the product fractions gave the desired product as a yellow oil (14.28 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07705005B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-c65d106b1848471aa9f779db620aa958 |
| Source note | uspto-grants-2010_04 |