関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| 反応物 | 3-[N-(2-cyclohexylethyl)amino]propionic acid hydrochloride | HCID 57440791 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-[N-(t-butoxycarbonyl)-N-(2-cyclohexylethyl)amino]propionic acid | HCID 12136624 | 62.8% |
反応手順
Next, tetrahydrofuran (8 ml) was added to 3-[N-(2-cyclohexylethyl)amino]propionic acid hydrochloride (1.0 g, 4.2 mmol), and the mixture was stirred at room temperature. Di-t-butyl carbonate (1.1 g, 5.1 mmol) and triethylamine (1.3 ml, 9.3 mmol) were added to the mixture, the whole was stirred overnight, and then a 5% aqueous citric acid solution (10 ml) was added to the reaction mixture. The whole was extracted with chloroform (60 ml), and the organic layer was washed with saturated brine (20 ml). The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 0.79 g (62%) of 3-[N-(t-butoxycarbonyl)-N-(2-cyclohexylethyl)amino]propionic acid as a colorless oily matter.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098226B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-7334d532e9ad4ab796ccc45ccdd76cb0 |
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| 出典メモ | uspto-grants-2006_08 |
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