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Sodium hydride → HCID 9967206、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 2-(2-Hydroxyethyl)-3-hydroxymethyl-5-pyridin-2-yl-4-quinolin-4-yl-pyrazole | HCID 21992612 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 9967206 | HCID 9967206 | — |
反応手順
To a solution of 2-(2-hydroxyethyl)-3-hydroxymethyl-5-pyridin-2-yl-4-quinoline-4-yl-pyrazole, (0.10 g, 0.29 mmol) in tetrahydrofuran (10 mL) cooled at 0° C. is added NaH (0.04 g, 50% in mineral oil). The mixture is stirred for 2 h at room temperature and methanesulfonyl chloride (0.065 g, 0.57 mmol) is added dropwise over 30 min. The reaction is quenched with water and extracted into ethyl acetate. The organic layer is washed with water, dried (sodium sulfate), filtered, and concentrated in vacuo. The residue is chromatographed on SiO2 (10% methanol/dichloromethane) to yield the title compound, 31 mg (33%), as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087626B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-be7a79edca974d11a6f6a3374a17c190 |
| 出典メモ | uspto-grants-2006_08 |