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Hydrochloric Acid → 4-(6-Chloro-1H-benzimidazol-2-yl)-6-(4-hydroxy-3,5-dimethylphenyl)-2H-pyridazin-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-[6-Chloro-1-(2-trimethylsilanylethoxymethyl)-1H-benzimidazol-2-yl]-6-(4-hydroxy-3,5-dimethyl phenyl)-2-(2-trimethylsilanylethoxymethyl)-2H-pyridazin-3-one | HCID 136343869 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(6-Chloro-1H-benzimidazol-2-yl)-6-(4-hydroxy-3,5-dimethylphenyl)-2H-pyridazin-3-one | HCID 135499851 | — |
反応手順
4-[6-Chloro-1-(2-trimethylsilanylethoxymethyl)-1H-benzimidazol-2-yl]-6-(4-hydroxy-3,5-dimethylphenyl)-2-(2-trimethylsilanylethoxymethyl)-2H-pyridazin-3-one is stirred in dichloromethane:trifluoroacetic acid/1:1 at RT for 30 min. The solvent is stripped off in vacuo, and the residue is dissolved in methanol, and 2M sodium hydroxide solution is added. The solution is stirred at RT for 30 min. After the reaction is complete, water is added and 2N hydrochloric acid is used for acidification. The precipitated product is filtered off with suction and purified by column chromatography (RP-HPLC, gradient of 0-100% acetonitrile in water (+0.01% trifluoroacetic acid)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07470689B2 |
| 出典データセット | uspto-grants-2008_12 |
| ORD ID | ord-75b39236e75547b281155d039bf1846e |
| 出典メモ | uspto-grants-2008_12 |