HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → 4-[4-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazin-1-yl]butan-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Methyl vinyl ketone | HCID 6570 | — |
| Reactant | 1-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazine | HCID 11992284 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 4-[4-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazin-1-yl]butan-2-one | HCID 23141548 | 78.6% |
Reaction Steps
A mixture of 1-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (160 mg, 0.532 mmol) produced in Example (8b), methyl vinyl ketone (0.058 mL, 0.692 mmol) and chloroform (0.7 mL) was stirred for 21 hours and 30 minutes at an external temperature of room temperature. The reaction mixture was diluted with ethyl acetate and then washed with aqueous solution of sodium hydrogencarbonate. The separated organic layer was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (ethyl acetate/heptane) to give 155 mg of the title compound as a light brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07425554B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-53ac3133cdaf40858950b2be4c8398f9 |
| Source note | uspto-grants-2008_09 |