関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | Methyl 4-(1-(tert-butoxycarbonyl)piperidin-4-yl)nicotinate | HCID 58442809 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 58442814 | HCID 58442814 | 67.6% |
反応手順
A solution of methyl 4-(1-(tert-butoxycarbonyl)piperidin-4-yl)nicotinate (2.6 g, 8.1 mmol, 1.0 eq.) in THF (50 mL) was added dropwise to a solution of lithium aluminium hydride (617 mg, 16.3 mmol, 2.0 eq.) in THF (100 mL) at 0° C. under nitrogen. The resulting solution was stirred for 0.5 hours while the temperature was maintained at 0° C. in an ice/salt bath. The reaction was then quenched with water (0.6 mL) and 15% NaOH (1.8 mL). The mixture was stirred for 10 minutes. The solids were filtered and washed with EtOAc (30 mL). The filtrate was dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was applied onto a silica gel column and eluted with EtOAc/MeOH (10:1) to yield the title compound (1.6 g) as a white solid. ES m/z: [M+H]+293.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530663B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-a5933b5ebfaf469f83ba3349ee302da9 |
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| 出典メモ | uspto-grants-2013_09 |
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