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Acetic Acid → 4-((4-Fluoro-1-(tetrahydro-2h-pyran-4-yl)piperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Tetrahydro-4H-pyran-4-one | HCID 121599 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | 4((4-Fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide | HCID 67126502 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-((4-Fluoro-1-(tetrahydro-2h-pyran-4-yl)piperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide | HCID 67126548 | — |
反応手順
A mixture of EXAMPLE 173A (0.4 g), dihydro-2H-pyran-4(3H)-one (0.179 g), sodium cyanoborohydride (0.112 g), and acetic acid (0.5 mL) in tetrahydrofuran (3 mL) was stirred overnight. The solvents were removed under reduced pressure. The residue was purified with flash column chromatography on silica gel eluting with 100:5:0.5 ethyl acetate/methanol/NH4OH to give the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09174982B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-248700d0e243479597c940a5d94380c2 |
| 出典メモ | uspto-grants-2015_11 |