関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 3-(3,5-Ditert-butyl-4-hydroxyphenyl)prop-2-enoic acid | HCID 99819 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | N-ethoxycarbonylmethylthioethyl-n-butylamine | HCID 86747655 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-ethoxycarbonylmethylthioethyl-N-n-butylcinnamamide | HCID 67822768 | 105% |
反応手順
First, 5.53 g of 3,5-di-t-butyl-4-hydroxycinnamic acid, 4.4 g of N-ethoxycarbonylmethylthioethyl-n-butylamine, and 4.0 g of 1-ethyl-3-(3dimethylaminopropyl)carbodiimide hydrochloride (WSC) were added to 100 ml of dichloromethane and the mixture was agitated for 3 hours at room temperature. Then, this reaction mixture was poured into water, and after chloroform extraction the chloroform layer was dehydrated with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue so obtained was separated and purified by column chromatography on silica gel with chloroform, after which hexane was added and crystallization yielded 7.34 g of an N-ethoxycarbonylmethylthioethyl-N-n-butylcinnamamide derivative (yield 79.5%) in the form of white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05294643 |
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| 出典データセット | uspto-grants-1994_03 |
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| ORD ID | ord-cfc51979bbf84a81b826fb784ea1f31d |
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| 出典メモ | uspto-grants-1994_03 |
|---|
