関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 2,5-Dibromo-3-nitropyridine | HCID 298470 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2,5-Dibromopyridin-3-amine | HCID 19387532 | 69.4% |
反応手順
To the solution of 2,5-Dibromo-3-nitro-pyridine (10.30 g, 35.47 mmol) in the 100 ml of ethanol was added SnCl2 (24.0 g, 106.42 mmol) slowly. The reaction mixture was heated at 80° C. for 2 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure. Water (250 mL) was added, white solid separated out, then, basified the reaction mixture with NaOH Solution. To this added the 250 ml of ethyl acetate. Filtered it and washed the residue with ethyl acetate, layers are separated, dried (Na2SO4), filtered, concentrated to give the desired product (6.20 g, 67.39%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088791B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-0b30792f287747c79386edfa93c9067f |
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| 出典メモ | uspto-grants-2012_01 |
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