HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Fluoropropyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 3-Fluoro-1-propanol | HCID 68042 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Fluoropropyl methanesulfonate | HCID 248388 | 91.6% |
Reaction Steps
A solution of 3-fluoro-propan-1-ol (31.2 g, 400 mmol) in 300 mL of CH2Cl2 was treated with methanesulfonyl chloride (55 g, 38 mL, 480 mmol, 1.2 equiv) at 0° C. The resulting reaction mixture was gradually warmed to room temperature and stirred for 1-2 hours. When 1H NMR showed the reaction was complete, the reaction mixture was treated with H2O (100 mL), and the two layers were separated. The aqueous layer was extracted with CH2Cl2 (2×100 mL). The combined organic layers were washed with H2O (3×100 mL) and dried over MgSO4. The solvent was removed in vacuo to afford the desired methanesulfonic acid 3-fluoro-propyl ester (57.2 g, 91% yield) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895741B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-7950e57dd2d04a54956cc3e31cfa68c5 |
| Source note | uspto-grants-2014_11 |