関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | Acetic acid (2-chloro-5-cyanothiophen-3-ylmethylene)hydrazide | HCID 68929248 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Diphenyl Ether | HCID 7583 | — |
| 生成物 | 1-Acetyl-1H-thieno[2,3-c]pyrazole-5-carbonitrile | HCID 68927237 | 10.1% |
反応手順
To a solution of 2.53 g of acetic acid (2-chloro-5-cyanothiophen-3-ylmethylene)hydrazide in 22 mL of diphenyl ether were added copper powder and potassium acetate at room temperature, and stirred at 200° C. for 6 hours. Following filtration through Celite, the filtrate was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10-1:5), to afford 215 mg of the title compound as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429609B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-9364f7cbd9224c62904bb2461f3a280e |
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| 出典メモ | uspto-grants-2008_09 |
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