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6-Thiophen-3-yl-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one → 4-(1H-Benzimidazol-2-yl)-6-thiophen-3-yl-2H-pyridazin-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-Thiophen-3-yl-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one | HCID 68680227 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 溶媒 | 1,1-Ethanedithiol | HCID 33645 | — |
| 生成物 | 4-(1H-Benzimidazol-2-yl)-6-thiophen-3-yl-2H-pyridazin-3-one | HCID 135978788 | — |
反応手順
30 mg of 6-thiophen-3-yl-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanyl -ethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one is dissolved in a mixture of dichloromethane (1 ml) and trifluoroacetic acid (1 ml), 18 μl of ethanedithiol are added, and the resulting solution is stirred at room temperature for 18 hours. After the solvent has been distilled off, the crude product is purified by preparative RP-HPLC (0-100% acetonitrile (+0.05% formic acid) in water (+0.05% formic acid)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07727989B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-a0bb0e36af1c4605afc2d9a01c94eb29 |
| 出典メモ | uspto-grants-2010_06 |