関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tyramine | HCID 5610 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | But-3-enoyl Chloride | HCID 10975427 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Vinylacetamidoethyl phenol | HCID 62679686 | 80% |
反応手順
A 1000 mL 3-neck, round bottom flask connected with a reflux condenser and a drying tube, is charged with 250 mL of methylene chloride, 5.48 grams (0.04 mole) 4-aminoethylphenol and 4.04 grams (0.04 mole) triethylamine. The contents are chilled with an ice bath. Through a dropping funnel, 4.18 grams (0.04 mole) of vinylacetyl chloride is added into the flask over a period of 30 minutes. The ice bath is then removed and the contents are continuously stirred overnight. The mixture is then filtered and then condensed using a rotavapor. HPLC analysis indicates only one major product. The product is then passed through silica gel chromatography to give a final purified product with a yield of at least 80 percent. The product is identified by NMR and Mass Spectroscopy.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07304117B2 |
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| 出典データセット | uspto-grants-2007_12 |
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| ORD ID | ord-10238c376db34c5086dacc7c295f9e36 |
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| 出典メモ | uspto-grants-2007_12 |
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