関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Mercaptobenzoic Acid | HCID 5443 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Iodoanisole | HCID 69676 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2-(4-Methoxyphenylthio)benzoic acid | HCID 2824878 | — |
反応手順
First, 2-(4-methoxyphenylthio)benzoic acid was prepared. A stirred mixture of thiosalicylic acid (10.0 g, 65 mmol), 4-iodoanisole (15.18 g, 65 mmol), potassium carbonate (19.72 g, 143 mmol), copper powder (0.82 g, 13 mmol), and N-methylpyrrolidinone (100 mL) was deaerated by sparging with nitrogen for 10 min, heated at 165° C. for 18 h, and then cooled to ambient. The reaction mixture was poured onto a mixture of 500 g of ice plus 40 mL or concentrated HCl. The resulting precipitate was collected, washed with water, and dried. The product was purified by recrystallization from a mixture of water, ethanol, and tetrahydrofuran. A white powder was obtained, mass: 12.06 g (71% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07459263B2 |
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| 出典データセット | uspto-grants-2008_12 |
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| ORD ID | ord-aff65ac74f8440e3ac3a2bece001f2f0 |
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| 出典メモ | uspto-grants-2008_12 |
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