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Borane;tetrahydrofuran → [3-Iodo-1-(tetrahydropyran-2-yl)-1H-pyrazol-4-yl]-methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 反応物 | 3-Iodo-1-(tetrahydro-pyran-2-yl)-1H-pyrazole-4-carboxylic acid | HCID 90424895 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | [3-Iodo-1-(tetrahydropyran-2-yl)-1H-pyrazol-4-yl]-methanol | HCID 90424555 | 83.5% |
反応手順
A solution of 3-iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxylic acid (34 g, 105 mmol) in BH3-THF (340 mL, 340 mmol, 1M in THF) was stirred at rt overnight. Solvent was evaporated under vacuum and the residue dissolved in DCM (340 mL), washed with water (340 mL×3), dried and concentrated. The residue was purified by SGC using Hex: EA (0%-70%) as eluent to afford (3-iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl)methanol (27 g, yield: 83%). LCMS (method C): RT=1.74 min, m/z=309.1 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09346761B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-09d32dd271d94ac29f9ab4c17ba5adf6 |
| 出典メモ | uspto-grants-2016_05 |