関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methylpyridine | HCID 7975 | — |
| 反応物 | 2,4-Dimethyl-3-pentanone | HCID 11271 | — |
| 反応物 | HCID 178418306 | HCID 178418306 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,4-Dimethyl-3-pyridin-2-ylmethyl-pentan-3-ol | HCID 16126274 | 99.8% |
反応手順
2-Methyl-pyridine (1.86 g, 20 mmol) is dissolved in THF (20 mL) and cooled to −30° C. tert-Butyl lithium (11.8 mL, 1.7M in pentane, 20 mmol) is added dropwise to the solution, and the reaction is stirred for 30 min at −30° C. 2,4-Dimethyl-pentan-3-one (3.4 mL, 24 mmol) is added and the reaction is warmed to room temperature and stirred for 2 h. Add H2O (30 mL) and extract with EtOAc. Wash combined organics with brine and concentrate in vacuo. The residue is purified by flash chromatography on silica gel (EtOAc/Heptane) to afford 2,4-dimethyl-3-pyridin-2-ylmethyl-pentan-3-ol (4.14 g, quant.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481542B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-afa77a35db864366800576026aaa111f |
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| 出典メモ | uspto-grants-2013_07 |
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