関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | O-Cresol | HCID 335 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-4-methoxybenzoic acid | HCID 66836 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 67076683 | HCID 67076683 | 53.7% |
反応手順
Potassium carbonate (1.20 g, 8.66 mmol), o-cresol (468 mg, 4.33 mmol), copper powder (28 mg, 0.43 mmol) and 3-bromo-4-methoxybenzoic acid (1.00 g, 4.33 mmol) were suspended in DMF (5 ml) and heated to 165° C. overnight. Potassium carbonate (1.20 g, 8.66 mmol) and o-cresol (468 mg, 4.33 mmol) were added once again and heating was continued for another 2 h. The crude mixture was partitioned between EA and 2 N hydrochloric acid, the aqueous phase extracted with EA, and the combined organic phases were dried over magnesium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel chromatography (HEP/EA gradient) to yield 600 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09328071B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-013c62593d8d4919bc487603c80ca7a4 |
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| 出典メモ | uspto-grants-2016_05 |
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