HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl Isobutyl Ketone → HCID 20278954, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl Isobutyl Ketone | HCID 7909 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 3-Chloro-1,1-diethoxypropane | HCID 96217 | — |
| Reactant | p-Fluorophenyl 4-piperidyl ketone hydrochloride | HCID 3084438 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20278954 | HCID 20278954 | 53% |
Reaction Steps
A mixture of 4.5 parts of 1-chloro-3,3-diethoxypropane, 12.15 parts of (4-fluorophenyl) (4-piperidinyl)methanone hydrochloride, 10.6 parts of sodium carbonate and 120 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure factors are collected and the eluent is evaporated. The residue is crystallized from a mixture of methylbenzene and 2,2'-oxybispropane, yielding 9 parts (53%) of [1-(3,3-diethoxypropyl)-4-piperidinyl] (4-fluorophenyl)methanone.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04335127 |
| Source dataset | uspto-grants-1982_06 |
| ORD ID | ord-37b587c9bac44d16b93bae20b281b4c7 |
| Source note | uspto-grants-1982_06 |