HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67402255, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 67401528 | HCID 67401528 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67402255 | HCID 67402255 | 83% |
Reaction Steps
4-Fluoro-4-[2,2,2-trifluoro-1-(triethylsiloxy)ethyl]-piperidine (300 mg, 0.951 mmol) was dissolved in dichloromethane (6 mL). To this, triethylamine (0.199 mL, 1.43 mmol) and methanesulfonyl chloride (0.140 mL, 1.43 mmol) were added and the mixture was stirred at room temperature for 30 minutes. The reaction was stopped by addition of water to the reaction mixture, and extraction with dichloromethane was performed, followed by drying over anhydrous sodium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=7/3) to give 4-fluoro-1-methanesulfonyl-4-[2,2,2-trifluoro-1-(triethyl-siloxy)ethyl]piperidine (309 mg, yield: 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673908B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-71f942cfe3e44520b4991451480df51b |
| Source note | uspto-grants-2014_03 |