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Toluene → N-[5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-yl]-4-(3,4-dimethylpiperazin-1-yl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 反応物 | 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine | HCID 57440381 | — |
| 反応物 | Ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate | HCID 57440404 | — |
| 生成物 | N-[5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-yl]-4-(3,4-dimethylpiperazin-1-yl)benzamide | HCID 66590060 | 43.1% |
反応手順
N-[5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-yl]-4-(3,4-dimethylpiperazin-1-yl)benzamide was prepared following the procedure for Example 100, but staring from ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.394 g, 1.50 mmol), 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine (0.374 g, 1.5 mmol) and 2M trimethylaluminium in toluene (1.875 mL, 3.75 mmol). The crude product was purified by silica column chromatography, eluting with a gradient of 0 to 5% 2M ammonia/MeOH in DCM. Pure fractions were evaporated to dryness to afford the title compound (0.301 g, 43.1%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08129391B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-74eac9c63bba43fd85bf3653f010d55a |
| 出典メモ | uspto-grants-2012_03 |