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Water → 2-[[3-Methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Iodobenzoic acid | HCID 6941 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine | HCID 735132 | — |
| 触媒 | Cupric acetate | HCID 8895 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[[3-Methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid | HCID 22320140 | 98% |
反応手順
A solution of 3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-ylamine (5.23 g, 30 mmol), o-iodobenzoic acid (8.93 g, 36 mmol), copper acetate (II) (0.654 g, 3.6 mmol), and potassium carbonate (4.98 g, 36 mmol) in N,N-dimethylformamide (30 mL) was heated under reflux for 1 hour under an argon atmosphere. After the solution was cooled to room temperature, the mixture was added to water. The solution was made weakly acidic by the addition of acetic acid, and the resulting crude crystals were collected by filtration. The crystals were washed with water and air dried to give the title compound (8.64 g, 98% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06949648B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-233acd72c0c449d7a0646a20355f0b60 |
| 出典メモ | uspto-grants-2005_09 |