化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Iodide → 3-Chloro-4-(thiazol-4-ylmethoxy)-phenylamine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Nitrofungin | HCID 12074 | — |
| 反応物 | 4-(Chloromethyl)-1,3-thiazole hydrochloride | HCID 2763289 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Chloro-4-(thiazol-4-ylmethoxy)-phenylamine hydrochloride | HCID 67313226 | 83% |
反応手順
To a solution of 2-chloro-4-nitrophenol (1.00 g, 5.76 mmol) in acetonitrile (125 mL) were added 4-chloromethylthiazole hydrochloride (1.08 g, 6.34 mmol), Potassium carbonate (2.39 g, 17.29 mmol) and sodium iodide (1.73 g, 11.52 mmol). The reaction mixture was stirred at 60 C overnight. Water (60 mL) and DCM (10 mL) were added. After all solid material dissolved, layers formed were separated. The organic layer was washed with water and brine, dried over Na2SO4 and concentrated down to give the required material as a light yellow solid (1.29 mg, 83%). 1H-NMR (CD2Cl2) δ 8.87 (d, 1H), 8.32 (d, 1H), 8.16 (dd, 1H), 7.54-7.56 (m, 1H), 7.22 (d, 1H), 5.33-5.34 (m, 2H); LCMS RT=3.01 min; [M+H]+=271.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07750017B2 |
| 出典データセット | uspto-grants-2010_07 |
| ORD ID | ord-d4aa5a7bbf1c42648a0fb93a0ecf77b8 |
| 出典メモ | uspto-grants-2010_07 |