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4-Aminotetrahydro-2H-pyran-4-carboxylic acid hydrochloride → Methyl 4-aminooxane-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminotetrahydro-2H-pyran-4-carboxylic acid hydrochloride | HCID 2734400 | — |
| 反応物 | trimethylsilyldiazomethane Et2O | HCID 23159941 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 4-aminooxane-4-carboxylate | HCID 18698314 | 99% |
反応手順
To a solution of 4-amino-4-carboxy-tetrahydropyrane hydrochloride (2 g) in methanol was added dropwise a solution of 2M trimethylsilyldiazomethane-diethylether (33 mL) under ice-cooling, and the mixture was stirred at room temperature for 4 days. The reaction mixture was concentrated in vacuo, and the resultant crude product was dissolved in hexane-diethylether (1 mL/1 mL), and thereto was added an aqueous 4N hydrochloric acid. The precipitates were collected by filtration to give 4-amino-4-methoxycarbonyl-tetrahydropyrane (2.13 g, yield: 99%) as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08921380B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-c6845010739e41f19e1c9c8429a37b52 |
| 出典メモ | uspto-grants-2014_12 |