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Methanol → 1-(4,5-dihydro-1H-imidazol-2-ylmethyl)-1H-indole-3-sulfonic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Trimethylsilyl chlorosulphate | HCID 78059 | — |
| 反応物 | 1-(4,5-Dihydro-1H-imidazol-2-ylmethyl)-1H-indole | HCID 22574001 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 1-(4,5-dihydro-1H-imidazol-2-ylmethyl)-1H-indole-3-sulfonic Acid | HCID 22574032 | — |
反応手順
1-(4,5-Dihydro-1H-imidazol-2-ylmethyl)-1H-indole (1.0 g, 4.243 mmol) was dissolved/suspended in dichloroethane (120 ml) and cooled in ice under a nitrogen atmosphere. Trimethylsilylchlorosulfonate (0.654 ml, 0.801 g, 4.243 mmol) was added to the cooled solution dropwise with stirring. The mixture was allowed to warm up to room temperature with stirring, and stirring was continued overnight. Methanol (20 mL) was then added, followed by stirring at room temperature for 20 minutes. The mixture was then rotovapped to dryness. The crude product was recrystallized from MeOH/EtOAc as the hydrochloride salt of 1-(4,5-dihydro-1H-imidazol-2-ylmethyl)-1H-indole-3-sulfonic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06852726B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-d6b16d7c07814c4788a5b54d5ffb8990 |
| 出典メモ | uspto-grants-2005_02 |