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Hydrochloric Acid → (S)-2-Benzenesulfonylamino-9-(5,6,7,8-tetrahydro-[1,8]naphthyridin-2-yl)-nonanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzenesulfinyl chloride | HCID 4190003 | — |
| 反応物 | 2-Amino-9-(5,6,7,8-tetrahydro-[1,8]naphthyridin-2-yl)-nonanoic acid | HCID 22678144 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | (S)-2-Benzenesulfonylamino-9-(5,6,7,8-tetrahydro-[1,8]naphthyridin-2-yl)-nonanoic acid | HCID 21967992 | — |
反応手順
A solution of 13-9 (0.27 g, 0.88 mmol) in H2O/dioxane (2:1, 4.4 mL) was cooled to 0° C. and then treated dropwise with 1N NaOH to attained a pH of 10.5. The reaction mixture was then treated with with PhSOCl (0.23 g, 1.3 mmol) in dioxane (750 μL) while maintaining a pH of 10.5 by adding 1N NaOH. After 15 min, the pH was adjusted to 7 with 1N HCl to effect a white precipitate. The precipitate was collected by filtration and triturated with EtOAc and then ether to give 13-10 as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06048861 |
| 出典データセット | uspto-grants-2000_04 |
| ORD ID | ord-b702bec4885e41419433bd0c88a315e9 |
| 出典メモ | uspto-grants-2000_04 |