HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 3-nitro-4-((tetrahydro-2H-pyran-4-yl)methoxy)benzenesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | (Oxan-4-yl)methanol | HCID 2773573 | — |
| Edukt | 4-Fluoro-3-nitrobenzenesulfonamide | HCID 16782487 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3-nitro-4-((tetrahydro-2H-pyran-4-yl)methoxy)benzenesulfonamide | HCID 67126458 | — |
Reaktionsschritte
(Tetrahydro-2H-pyran-4-yl)methanol (2.0 g) in tetrahydrofuran (20 mL) was treated with 60% NaH (1.377 g). The mixture was stirred for 20 minutes at the room temperature. To this mixture was added 4-fluoro-3-nitrobenzenesulfonamide (2.84 g) portionwise. The reaction was stirred for another 2 hours. The mixture was poured into water, neutralized with 10% HCl, and extracted with ethyl acetate three times. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated. The residue was purified with flash column chromatography on silica gel eluting with 20%-60% ethyl acetate in hexanes.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09315488B2 |
| Quelldatensatz | uspto-grants-2016_04 |
| ORD ID | ord-5c1bb051f1fa47e3a8c3171b1a8d5c25 |
| Quellennotiz | uspto-grants-2016_04 |