HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67401456, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 67402546 | HCID 67402546 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67401456 | HCID 67401456 | 79% |
Reaction Steps
4-[2,2,2-Trifluoro-1-(triethylsiloxy)ethyl]piperidine (303 mg, 1.02 mmol) was dissolved in dichloromethane (6 mL). To this, triethylamine (0.213 mL, 1.53 mmol) and methanesulfonyl chloride (0.118 mL, 1.53 mmol) were added at 0° C. 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=4/1) to give 1-methanesulfonyl-4-[2,2,2-trifluoro-1-(triethylsiloxy)-ethyl]piperidine (302 mg, yield: 79%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673908B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-c0aa31c6781140a9b2f0cc159e94d3f8 |
| Source note | uspto-grants-2014_03 |