関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Ethyl 2-(5-((tert-butyldiphenylsilyloxy)methyl)-4-((2R,6S)-2,6-dimethylmorpholino)-2,3-difluorophenyl)-2-oxoacetate | HCID 86658065 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 86658093 | HCID 86658093 | — |
反応手順
Ethyl 2-(5-((tert-butyldiphenylsilyloxy)methyl)-4-((2R,6S)-2,6-dimethylmorpholino)-2,3-difluorophenyl)-2-oxoacetate (Intermediate 114, 2.808 g, 4.71 mmol) and hydroxylamine hydrochloride (0.360 g, 5.18 mmol) were dissolved in pyridine (40 ml) and stirred at 115° C. for 16 hours. The reaction was concentrated to remove excess pyridine. The residue was dissolved in ethyl acetate and washed with water and brine 3×. The organic layer was dried over MgSO4 and concentrated. The residue was purified by silica gel column chromatography using a gradient of hexanes to ethyl acetate to give the title compound as a mixture of oxime isomers (1.924 g, 3.15 mmol, 66.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09040528B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-1ef981f6283f4f9eba78355e90d7ce2b |
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| 出典メモ | uspto-grants-2015_05 |
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