HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (Tetrahydrofuran-3-yl)methyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Tetrahydro-3-furanmethanol | HCID 139980 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (Tetrahydrofuran-3-yl)methyl methanesulfonate | HCID 22273010 | 99% |
Reaction Steps
To a stirring solution of (3-oxolanyl)methan-1-ol (25 g, 245 mmol) and triethylamine (34.37 mL, 245 mmol) in dry dichloromethane (250 mL) at 0° C. under N2 atmosphere was added dropwise methanesulfonyl chloride (18.94 mL, 245 mmol). The reaction mixture was stirred overnight after warming to room temperature, then a saturated solution of NaHCO3 (100 mL) was added and the mixture stirred for another 30 min. The biphasic mixture was separated and the organic layer was discarded. The aqueous layer was extracted with dichloromethane (3×25 mL) and the combined dichloromethane extracts were dried (Na2SO4), filtered and concentrated by rotary evaporation to give 42.16 g of (3-oxolanyl)methyl methanesulfonate (99%) as a light brown liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07291731B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-91b0cf3302cb452b9fc7c35985af58b8 |
| Source note | uspto-grants-2007_11 |