関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Furfuryl Alcohol | HCID 7361 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 反応物 | Methyl 1-aminocyclohexanoate | HCID 4048819 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-[[(2-Furanylmethoxy)carbonyl]amino]cyclohexanecarboxylic acid methyl ester | HCID 57672888 | 88.1% |
反応手順
3.67 g (30 mmol) of dimethylaminopyridine was added to a solution of 65.48 g (0.3 mol) of di-t-butyl dicarbonate in 300 ml of anhydrous toluene, and the mixture was stirred at room temperature for 15 minutes. A solution of 47.17 g (0.3 mol) of 1-aminocyclohexanecarboxylic acid methyl ester in 100 ml of anhydrous toluene was added to the reaction solution, and the mixture was stirred at room temperature for 1 hour. Further, after 60.71 g (0.6 mol) of triethylamine and 44.1 g (0.45 mol) of furfuryl alcohol were added, the mixture was heated under reflux for 3 hours. The reaction solution was returned to room temperature and was concentrated under reduced pressure. The obtained residue was crushed by a mortar, and it was stirred in a mixture solution of 5 ml of hydrochloric acid and 3 L of water for 18 hours. The obtained crystal was collected by filtration to obtain 74.37 g (88%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481725B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-7cbbf8d9e18e419fbc2b42a30e8de1e8 |
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| 出典メモ | uspto-grants-2013_07 |
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