HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2,2-Difluoropropyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 2,2-Difluoropropanol | HCID 13394818 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2,2-Difluoropropyl methanesulfonate | HCID 87317344 | 75% |
Reaction Steps
To a mixture of 2,2-difluoropropan-1-ol (2.00 g, 20.8 mmol) and TEA (3.16 g, 31.25 mmol) in dry DCM (20 mL) was added methanesulfonyl chloride (2.84 g, 24.96 mmol) at 0° C. The resulting reaction mixture was stirred at rt for 1.5 h. Water was added and the mixture was extracted with DCM (3×100 mL). The combined organic layers were washed with saturated aqueous ammonium chloride solution, brine, dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated under vacuum to give the title product (2.70 g, 15.52 mmol, 75% yield), which was used directly in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156798B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-0a0db1c494e64128832c448b6fb7ef41 |
| Source note | uspto-grants-2015_10 |