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Water → 1H-Benzoimidazole-2-carboxylic acid [4-(4-oxo-4H-pyridin-1-yl)-phenyl]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzimidazole, 2-trichloromethyl- | HCID 77133 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-(4-Amino-phenyl)-1H-pyridin-4-one | HCID 57437533 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1H-Benzoimidazole-2-carboxylic acid [4-(4-oxo-4H-pyridin-1-yl)-phenyl]-amide | HCID 86761132 | — |
反応手順
A solution of 769 mg 2-Trichloromethyl-1H-benzoimidazole in 10 mL THF were slowly added to a mixture containing 304 mg 1-(4-Amino-phenyl)-1H-pyridin-4-one, 1.3 g NaHCO3, 40 mL THF and 15 mL H2O. The mixture was stirred vigorously for 3 h at room temperature, diluted with 200 mL CH2Cl2 and washed with 40 mL of a saturated NaHCO3-solution. The aqueous solution was extracted with CH2Cl2 (3×200 ml) and the combined organic layers were dried over MgSO4 and concentrated under reduced pressure to give a brown solid, which was pure enough for the following reactions.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741341B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-ce1eae390e274e7aaf0ec5c11672db47 |
| 出典メモ | uspto-grants-2010_06 |