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Hydroxyamine hydrochloride → 4-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyiminomethyl]-piperidine-1-carboxylic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 4-(2-Fluoro-5-trifluoromethyl-benzoyl)-piperidine-1-carboxylic acid tert-butyl ester | HCID 58817544 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyiminomethyl]-piperidine-1-carboxylic acid tert-butyl ester | HCID 72434547 | — |
反応手順
A solution of 4-(2-fluoro-5-trifluoromethyl-benzoyl)-piperidine-1-carboxylic acid tert-butyl ester (59, 0.013M) in pyridine (25 mL) was treated with hydroxylamine hydrochloride (1.11 g, 0.015 M-1.2 eq). The reaction was stirred under N2 at room temperature for 14 hours and then poured onto ice water (250 mL). The mixture was stirred at 0° C. for 1 hour, the product was then filtered off, washed with cold water (3×15 mL) and dried in a vacuum oven at 50° C. A white solid was obtained (5.03 g, 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07772252B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-d3befe8109454906845c3d380e924555 |
| 出典メモ | uspto-grants-2010_08 |