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Azobisisobutyronitrile → 3-Methoxy-2-nitro-6-pyridylmethyl bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 3-Methoxy-6-methyl-2-nitropyridine | HCID 2727965 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 3-Methoxy-2-nitro-6-pyridylmethyl bromide | HCID 14405124 | 21.3% |
反応手順
A catalytic amount of α,α'-azobis(isobutyronitrile) was added to 3-methoxy-6-methyl-2-nitropyridine (described in Acta Chem. Scand., vol. 23, pages 1791-1796) (7.1 g), N-bromosuccinimide (7.1 g) and carbon tetrachloride (80 ml), and the mixture was refluxed for 16 hours. After the reaction, while the reaction mixture was still hot, it was suction-filtered to separate the insoluble succinimide. The filtrate was cooled to room temperature whereupon the unreacted 3-methoxy-6-methyl-2-nitropyridine precipitated as crystals. The crystals were separated by filtration. The residue was concentrated and then vacuum distilled to give 3-methoxy-2-nitro-6-pyridylmethyl bromide (2.1 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04772620 |
| 出典データセット | uspto-grants-1988_09 |
| ORD ID | ord-f9c7e3be90e044b4ae9244e313e2dd74 |
| 出典メモ | uspto-grants-1988_09 |