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Hydrochloric Acid → 1-(6-Acetylenyl-2-benzothiazolyl)-3-ethylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-(6-Trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea | HCID 21985542 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(6-Acetylenyl-2-benzothiazolyl)-3-ethylurea | HCID 21985592 | 5.6% |
反応手順
A mixture of 1-(6-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea (0.0710 g, 0.22 mmol) and 1M aqueous KOH solution (1.22 mL, 1.22 mmol, 5.5 eq) in 1.5 mL MeOH was stirred at room temperature for about 2 hours. The mixture acidified with 1 M HCl, then taken up in 20 mL AcOEt, and the aqueous phase was extracted with 10 mL AcOEt. The combined organic portions were dried (MgSO4), concentrated, and purified by HPLC to give the desired compound 0.003 g (5%). LC/MS 246 (M+1); LC retention time 2.84 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091227B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-e28f5a27454f477e9bdcf8a67a519fdf |
| 出典メモ | uspto-grants-2006_08 |