関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Aminosalicylic Acid | HCID 4649 | — |
| 反応物 | 2,6-Octadiene, 1-bromo-3,7-dimethyl-, (2E)- | HCID 5365867 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-{(2E)-3,7-dimethylocta-2,6-dienyl}-4-amino-2-hydroxybenzoic acid | HCID 69130364 | 7.6% |
反応手順
In 30 ml of DMF was dissolved 2.12 g (13.8 mmol) of 4-amino-2-hydroxybenzoic acid, and 3.0 g (13.8 mmol) of geranyl bromide was added thereto. After the mixture was stirred at room temperature for 4 hours, water was added thereto, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated sodium chloride aqueous solution, dried over anhydrous sodium sulfate, and concentrated. The resulting crude product was purified by column chromatography and recrystallized from ethyl acetate/hexane to obtain 0.30 g (yield: 7.6%) of N-{(2E)-3,7-dimethylocta-2,6-dienyl}-4-amino-2-hydroxybenzoic acid represented by the following structural formula (hereinafter referred to as compound 47) as white crystals. The analytical results are shown below. ##STR68##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05646184 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-5316f008abab4fd7b2c48ac561965c04 |
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| 出典メモ | uspto-grants-1997_07 |
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