関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-Benzofuran-5-carbohydrazide | HCID 68664129 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178527940 | HCID 178527940 | 36% |
反応手順
To a solution of 1-benzofuran-5-carbohydrazide (1.50 g, 8.51 mmol) in ethanol (60 mL) were added potassium hydroxide (0.72 g, 12.8 mmol) and carbon disulfide (15.3 mL, 25.5 mmol), and the resulting mixture was stirred at room temperature for 5 hr. The reaction mixture was concentrated under reduced pressure, a mixture of the residue and N,N-dimethylformamide (30 mL) was tightly sealed in a vial, and the microwave was irradiated at 150° C. for 1 min. After cooling, the reaction mixture was acidified with 1M hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from hexane/ethyl acetate to give the title compound (0.66 g, yield 36%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08492378B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-b92e4429247045c6bb8017f35dc52523 |
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| 出典メモ | uspto-grants-2013_07 |
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