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Hydrochloric Acid → 4-cyano-7-fluoro-N,5-dimethyl-6-phenyl-N-(2-phenylethyl)-1,3-benzoxazole-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N-Methylbenzeneethanamine | HCID 11503 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 反応物 | Ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate | HCID 51041426 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-cyano-7-fluoro-N,5-dimethyl-6-phenyl-N-(2-phenylethyl)-1,3-benzoxazole-2-carboxamide | HCID 68585078 | — |
反応手順
Under nitrogen atmosphere, trimethylaluminium (1.03 M n-hexane solution, 1.80 ml, 1.85 mmol) was dropwise added at room temperature to a dichloromethane (3 ml) solution of N-methylphenethylamine (269 μl, 1.85 mmol), and stirred for 25 minutes. Subsequently, a dichloromethane (3 ml) solution of ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate (I-111) (300 mg, 925 μl) was dropwise added and stirred for 14.5 hours. After the reaction, aqueous 1 N hydrochloric acid solution was added to the reaction liquid with cooling with ice, followed by stirring at room temperature, and the reaction liquid was extracted with chloroform.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737166B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-3c23cc3f34664b59a15fc35c79f1eae3 |
| 出典メモ | uspto-grants-2010_06 |