HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tetrahydrofuran → (5-Chloropyridin-2-yl)methyl methanesulfonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Methanesulfonyl chloride | HCID 31297 | — |
| Edukt | (5-Chloropyridin-2-yl)methanol | HCID 20537893 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | (5-Chloropyridin-2-yl)methyl methanesulfonate | HCID 70700476 | 99% |
Reaktionsschritte
Triethylamine (12 mL) and methanesulfonyl chloride (5.7 mL) were added to tetrahydrofuran (150 mL) solution of 5-chloro-2-hydroxymethylpyridine (12.77 g) under cooling with ice, and stirred for 30 minutes under cooling with ice. After addition of water (150 mL), the reaction liquid was extracted with ethyl acetate (150 mL+150 mL), and the organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was crystallized from ethyl acetate-diisopropyl ether mixed solvent to provide the title compound (14.65 g, 99%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07732456B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-9a5fbfe159bf429d946f028309c04113 |
| Quellennotiz | uspto-grants-2010_06 |