関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 1-(2,2-dimethylpropanoyl)piperidine-4-carboxylate | HCID 1164515 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [1-(2,2-Dimethylpropyl)piperidin-4-yl]methanol | HCID 21060224 | 97% |
反応手順
20a (29.5 g, 122 mmol) was dissolved in 200 mL of tetrahydrofuran and cooled to 0° C. Lithium aluminum hydride (s) (10.6 g, 279 mmol) was added slowly and the reaction was allowed to warm to rt and stirred for 24 h. The reaction was quenched by slow addition of sodium sulfate hydrated crystals (Na2SO4.10H2O) until there was no bubbling on addition followed by 20 mL of water. The mixture was filtered through Celite®, and the Celite® washed with diethyl ether. The solvent was removed from the filtrate to provide 20 g (97%) of the desired product as a white solid. 1H NMR (400 MHz, CDCl3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728008B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-cc3d8336b3cb4a12933dd1ca2bc5b351 |
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| 出典メモ | uspto-grants-2010_06 |
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