関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 4-Iodotoluene | HCID 12207 | — |
| 反応物 | 2-Aminoterephthalic acid | HCID 2724822 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | 2,3-Butanediol | HCID 262 | — |
| 生成物 | HCID 59019548 | HCID 59019548 | — |
反応手順
To a mixture of 2-amino-terephthalic acid (2.5 g, 23.8 mmol) and 1-iodo-4-methyl-benzene (7.78 g, 35.7 mmol) in butane-2,3-diol (38 mL) was added Cu (24 mg, 0.016 mmol), CuCl (950 mg, 9.6 mmol), and n-methyl morpholine (6.5 mL) under argon. The mixture was heated at 150° C. for 18 h. The reaction mixture was cooled to room temperature and HCl (0.1 N, 100 mL) was added. The resulting yellow precipitate was collected by filtration and triturated in a mixture of Et2O and EtOAc (1:1, 50 mL) for 1 h. The yellow solid was filtered, washed with ether (25 mL), and dried in vacuo to give 2.4 of 138A. HPLC retention time=3.046 min., condition A.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07312209B2 |
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| 出典データセット | uspto-grants-2007_12 |
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| ORD ID | ord-47cc4bc63a3c4d10875cfc204faaee5e |
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| 出典メモ | uspto-grants-2007_12 |
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