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1-Hydroxybenzotriazole → 2-[2-(4-Chloro-2-fluoro-phenyl)-acetylamino]-benzothiazole-6-carboxylic acid (2-oxo-2,3-dihydro-benzooxazol-6-yl)-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 6-amino-1,3-benzoxazol-2(3H)-one | HCID 826989 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 2-[2-(4-Chloro-2-fluoro-phenyl)-acetylamino]-benzothiazole-6-carboxylic acid | HCID 86661382 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[2-(4-Chloro-2-fluoro-phenyl)-acetylamino]-benzothiazole-6-carboxylic acid (2-oxo-2,3-dihydro-benzooxazol-6-yl)-amide | HCID 46940548 | 24% |
反応手順
Starting material 37 (60 mg, 0.2 mmol, 70% content) and 6-Amino-3H-benzooxazol-2-one (30, 25 mg, 0.2 mmol) were dissolved in 2 ml DMF. Then EDCl (38 mg, 0.2 mmol) and HOBt (31 mg, 0.2 mmol) were added. The reaction was stirred over night at ambient temperature, concentrated in vacuo and purified by prep HPLC (Method 1). By concentration of the pure fractions the desired product 38 (23 mg, 0.04 mmol, 24%) could be isolated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08497283B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-8d817f441e4c481f9302ba7614b06267 |
| 出典メモ | uspto-grants-2013_07 |