HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 14576905, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 14576866 | HCID 14576866 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 14576905 | HCID 14576905 | 95.3% |
Reaction Steps
To a stirred mixture of 7.7 g of 1-(4-chlorophenyl)-6-(4-methylthiophenyl)-2-piperidone, 80 ml of methylene chloride, 3 g of silica gel, and 2.2 g of water was added 3.44 g of sulfuryl chloride at 15° to 25° C., and the mixture was stirred at 15° to 25° C. for 2 hours. The reaction mixture was poured into a cold aqueous sodium hydrogen carbonate solution. The methylene chloride solution was washed with a saturated aqueous sodium chloride solution, dried, and concentrated. The residue was purified by silica gel column chromatography (solvent; ethyl acetate:ethanol=10:1) and recrystallization from ethyl acetate to give 7.69 g of 1-(4-chlorophenyl)-6-(4-methylsulfinylphenyl)-2-piperidone as colorless prisms.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04839360 |
| Source dataset | uspto-grants-1989_06 |
| ORD ID | ord-1fd930e5bbe74d2386236d9e86aeb794 |
| Source note | uspto-grants-1989_06 |