関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Chlorothiophenol | HCID 16257 | — |
| 反応物 | 2-Bromo-5-methoxybenzoic acid | HCID 89906 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-[(3-Chlorophenyl)thio]-5-methoxybenzoic acid | HCID 341153 | 67.9% |
反応手順
To a mixture of 3-chlorothiophenol (20 g, 0.138 mol), and cupric acetate (1.8 g) and DMF (200 mL) was added K2CO3 (23 g). The mixture was heated to 150° C. for 15-20 minutes, then 2-bromo-5-methoxybenzoic acid (35.8 g, 0.155 mol) was added in portions. The mixture was heated overnight, poured into water (600 mL), filtered and the filtrate was treated with charcoal, filtered and diluted with HCl. The resulting precipitate was collected by filtration, washed with water, and dried at 50° C. in vacuo over P2O5 to afford 27.6 g of 2-[(3-chlorophenyl) thio]-5-methoxybenzoic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05380749 |
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| 出典データセット | uspto-grants-1995_01 |
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| ORD ID | ord-5954937a007e44a4a44183c074f0b0b5 |
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| 出典メモ | uspto-grants-1995_01 |
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