HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-Methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 6,6,7,7,7-Pentafluoroheptan-1-ol | HCID 12017063 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane | HCID 12017064 | 82.1% |
Reaction Steps
Triethylamine (25.83 ml, 185.3 mmol) and methanesulfonyl chloride (6.9 ml, 88.9 mmol) were added dropwise to a solution of 6,6,7,7,7-pentafluoroheptan-1-ol (14.1 g, 74.1 mmol) in dichloromethane (350 ml) at 0° C., followed by stirring for 1 hour. After the reaction was completed, water was added to the reaction mixture, which was then extracted twice with dichloromethane. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/10) to give 1-methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane (17.3 g, Yield 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06552068B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-cdd26ddf1c6246c7864ac58b959853a6 |
| Source note | uspto-grants-2003_04 |