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Phosphorus oxychloride → N-[4-(2-dimethylaminomethyl-phenyl)-2-fluorophenyl]-2-(2-fluorophenyl)-2-(4-chlorophenylaminocarbonylamino)-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 4-(2-Dimethylaminomethyl-phenyl)-2-fluoro-phenylamine | HCID 17978162 | — |
| 反応物 | 2-(2-Fluorophenyl)-2-(4-chlorophenylaminocarbonylamino)-acetic acid | HCID 68695741 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-[4-(2-dimethylaminomethyl-phenyl)-2-fluorophenyl]-2-(2-fluorophenyl)-2-(4-chlorophenylaminocarbonylamino)-acetamide | HCID 11713702 | 24.7% |
反応手順
To a solution of 2-(2-fluorophenyl)-2-(4-chlorophenylaminocarbonylamino)-acetic acid (from EXAMPLE 55, 90 mg, 0.28 mmol) and 4-(2-dimethylaminomethyl-phenyl)-2-fluoro-phenylamine (80 mg, 0.33 mmol) in pyridine (3 mL) cooled in an ice-bath, POCl3 (0.050 mL, 0.55 mmol) was added. After being stirred at room temperature overnight, the mixture was concentrated in vacuo. The residue was purified by HPLC to give the titled compound as a powder (38 mg). MS 549.1 and 551.2 (M+H, Cl pattern).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07678913B2 |
| 出典データセット | uspto-grants-2010_03 |
| ORD ID | ord-7df17864253f440590ce2bea7bee265c |
| 出典メモ | uspto-grants-2010_03 |