HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Toluenesulfonyl chloride → (Oxan-3-yl)methyl 4-methylbenzene-1-sulfonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Edukt | Tetrahydro-2H-pyran-3-methanol | HCID 85769 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | (Oxan-3-yl)methyl 4-methylbenzene-1-sulfonate | HCID 86618913 | — |
Reaktionsschritte
To a solution of (tetrahydropyran-3-yl)-methanol (Matrix, 1.67 g, 14.4 mmol) in 15 mL of CH2Cl2 and 15 mL of pyridine was added p-toluenesulfonyl chloride (2.9 g, 15.1 mmol) in portions over 10 minutes. The mixture stirred at ambient temperature for 18 hours and was quenched with 10 mL of saturated, aqueous NaHCO3. The layers were separated and the aqueous phase was extracted three 5 mL of portions of CH2Cl2. The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. Purification via column chromatography (SiO2, 70% hexanes in ethyl acetate) afforded the title compound. MS (DCI/NH3) m/z 288 (M+NH4)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08841334B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-25715a1446204b478a238d2771de1968 |
| Quellennotiz | uspto-grants-2014_09 |