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Dimethylacetamide → 5-Bromo-3-nitropyridine-2-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 2,5-Dibromo-3-nitropyridine | HCID 298470 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Bromo-3-nitropyridine-2-carbonitrile | HCID 2769698 | — |
反応手順
Heat a solution of 2,5-dibromo-3-nitropyridine (1.77 g, 6.3 mmol; Malinowski (1988) Bull. Soc. Chim. Belg. 97:51; see also U.S. Pat. No. 5,801,183) and cuprous cyanide (0.60 g, 6.69 mmol) in N,N-dimethylacetamide (25 mL) at 100° C. for 72 hours. After cooling, dilute the mixture with water (25 mL) and extract twice with EtOAc (25 mL each), then wash twice with water (25 mL each). The combined EtOAc extracts are dried (Na2SO4), evaporated, and purified by flash chromatography (50% EtOAc-hexane) to obtain 5-bromo-3-nitropyridine-2-carbonitrile as a pale solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07304059B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-794d4594877541a581123f5d48253418 |
| 出典メモ | uspto-grants-2007_12 |