HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Oxan-4-ylmethyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | (Oxan-4-yl)methanol | HCID 2773573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Oxan-4-ylmethyl methanesulfonate | HCID 15166436 | 96% |
Reaction Steps
To a solution of (IV) (1.25 g, 10.78 mmol) in dry THF (20 mL) at 0° C. under a nitrogen atmosphere was added triethyl amine (2.26 mL, 16.17 mmol) followed by methanesulfonyl chloride (1.0 mL, 12.94 mmol). The ice bath was removed and the reaction mixture was stirred for and additional 2 hours. Sodium bicarbonate (10% aq., 20 mL) was then added to the reaction mixture followed by extraction with ethyl acetate (3×20 mL). Combined organic extracts were then dried over anhydrous potassium carbonate. Filtration, followed by evaporation of solvents on a rotary evaporator yielded the mesylate (V) as a yellow oil (2.01 g, 96% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05559124 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-98eeaf22bf70466081a2c4dc1b508a17 |
| Source note | uspto-grants-1996_09 |