化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 3-nitro-4-((tetrahydro-2H-pyran-4-yl)methoxy)benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (Oxan-4-yl)methanol | HCID 2773573 | — |
| 反応物 | 4-Fluoro-3-nitrobenzenesulfonamide | HCID 16782487 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-nitro-4-((tetrahydro-2H-pyran-4-yl)methoxy)benzenesulfonamide | HCID 67126458 | — |
反応手順
(Tetrahydro-2H-pyran-4-yl)methanol (2.0 g) in tetrahydrofuran (20 mL) was treated with 60% NaH (1.377 g). The solution was stirred for 20 minutes at room temperature. To this solution was added 4-fluoro-3-nitrobenzenesulfonamide (2.84 g) portion-wise. 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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029404B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-7a9bf0e0bdd24129b52664f20749d9f3 |
| 出典メモ | uspto-grants-2015_05 |