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Benzothiazole-6-carboxylic acid → N'-[3-[3-(trifluoromethyl)phenyl]propionyl]benzothiazole-6-carbohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzothiazole-6-carboxylic acid | HCID 601670 | — |
| 反応物 | 3-[3-(Trifluoromethyl)phenyl]propanohydrazide | HCID 68663587 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N'-[3-[3-(trifluoromethyl)phenyl]propionyl]benzothiazole-6-carbohydrazide | HCID 68664426 | 67% |
反応手順
To a solution of benzothiazole-6-carboxylic acid (358 mg, 2.00 mmol) in tetrahydrofuran (10 mL) was added N,N′-carbonyldiimidazole (341 mg, 2.10 mmol) at room temperature, and the resulting mixture was stirred for 1 hr. To this reaction mixture was added 3-[3-(trifluoromethyl)phenyl]propanohydrazide (557 mg, 2.40 mmol), and the mixture was further stirred at room temperature for 24 hr. The reaction mixture was concentrated under reduced pressure, and ethyl acetate was added to the residue. The precipitate was collected by filtration, purified by basic silica gel column chromatography (tetrahydrofuran) and recrystallized from hexane/tetrahydrofuran to give the title compound (524 mg, yield 67%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08492378B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-a3a0ed6e055a466d858007180ec4798e |
| 出典メモ | uspto-grants-2013_07 |