関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dibromomethane | HCID 3024 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,4-Dihydroxybenzonitrile | HCID 87065 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzo-1,3-dioxole-5-carbonitrile | HCID 78136 | 94.8% |
反応手順
To a solution of 3,4 Dihydroxy benzonitrile (5.0 g, 37.0 mmol) in 20 ml of DMF was added dibromomethane (19.25 g, 110.0 mmol) and potassium carbonate (25.50 g, 184.90 mmol). The reaction mixture was heated at 120° C. for 2 h under the nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), reaction mixture was cooled to room temperature. Water (50 ml) was added to the reaction mixture and extracted the compound with ethyl acetate (3×100 mL). The combined organic layers were dried over anhydrous Na2SO4, and evaporated to dryness under reduced pressure to give the title compound as yellow solid (5.16 g, 94.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08865736B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-dac97f44beb24917a37737a85db83b1b |
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| 出典メモ | uspto-grants-2014_10 |
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