関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Hydroxybenzoic Acid | HCID 135 | — |
| 反応物 | 2-Fluoro-4-hydroxybenzoic Acid | HCID 2783398 | — |
| 反応物 | 4-(Chlorocarbonyl)phenyl decanoate | HCID 54563049 | — |
| 生成物 | Benzoic acid, 4-(acetyloxy)- | HCID 16865 | — |
反応手順
p-Acetoxybenzoic acid was prepared in the same manner as in Example 1(2) except that the 2-fluoro-4-hydroxybenzoic acid was replaced with p-hydroxybenzoic acid. The p-hydroxybenzoic acid was chlorinated in the same manner as in the above (2), to obtain an acid chloride. 1.8 Grams of the acid chloride and 2 g of the (R)-(+)-2-fluoro-4-hydroxy-1-(1-trifluoromethyl-6-ethoxyhexyloxycarbonyl)benzene obtained in Example 1 were dissolved in 50 ml of toluene, 6 ml of pyridine was added, and the mixture was stirred for 1 day. The reaction mixture was poured into water, consecutively washed with a hydrochloric acid aqueous solution, with a sodium hydroxide aqueous solution and with water, and dried over anhydrous sodium sulfate, and the solvent was distilled off to give a crude product. The crude product was purified by silica gel column chromatography(eluting solvent: ethyl acetate/hexane=15/85), to give 2.8 g of an end product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05723069 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-d965967cbe69411f9fd760ac1f990dfb |
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| 出典メモ | uspto-grants-1998_03 |
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