関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 3-(3-Hydroxy-4-methoxyphenyl)prop-2-enoic acid | HCID 92126 | — |
| 反応物 | 4-Aminoazepan-2-one | HCID 21584138 | — |
| 生成物 | 3-(4-Ethoxycarbonyloxycinnamoyl)amino-epsilon-caprolactam | HCID 53856471 | — |
反応手順
Ethyl chloroformate (22.2 ml) was added dropwise to a mixture of 3-hydroxy-4-methoxycinnamic acid (22.5 g), triethylamine (32.3 ml) and THF (400 ml) under ice-cooling and stirring, followed by stirring for 15 mins. Subsequently, to the mixture was added dropwise a solution of 3-amino-ε-caprolactam (14.9 g) in THF (200 ml), and then the whole was stirred for 1 hr. at room temperature. After completing the dropping, the reaction mixture was concentrated under reduced pressure, and the residue was dissolved in chloroform. This solution was washed with water, dried and distilled under reduced pressure to remove the solvent. The residue was washed with ethyl acetate, dried under reduced pressure to give the title compound (28 g). This compound was used in the following reaction without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05118806 |
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| 出典データセット | uspto-grants-1992_06 |
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| ORD ID | ord-2f7299906dbe4a1e92167c16c3c5d7ce |
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| 出典メモ | uspto-grants-1992_06 |
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