関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Bromo-2,5-dichloro-4-nitrobenzene | HCID 21190016 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(5-Bromo-4-chloro-2-nitrophenyl)glycine | HCID 10063959 | — |
反応手順
To a stirred solution of 4-bromo-2,5-dichloronitrobenzene (1.000 g, 3.691 mmol) in DMF (10.0 mL) at 65° C. was added dropwise a solution of NaHCO3 (0.316 g, 3.76 mmol) and glycine (0.280 g, 3.73 mmol, Aldrich, used as received) in water (3.8 mL). The resulting suspension was stirred at 65° C. for 65 h. The bright orange suspension was then cooled to r.t., filtered, washed with water (1.0 mL) and dried under vacuum to afford 0.284 g (98%, based on recovered starting material) of pure title compound as an orange powder; m.p. 264°-265° C. (decomposed); 1H NMR (DMSO-d6): 3.451 (d, 2H, J=3.9 Hz), 7.199 (s, 1H), 8.130 (s, 1H), 8.793 (t, 1H, J=3.6 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05620979 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-285f07f5c0544f158ded0aeafcdc2fdb |
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| 出典メモ | uspto-grants-1997_04 |
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