関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| 反応物 | 3-Methyl-5-nitropicolinonitrile | HCID 12404040 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Cyano-3,4-dimethyl-5-nitropyridine | HCID 21875209 | 42.3% |
反応手順
2-Cyano-3-methyl-5-nitropyridine (0.33g, 2 mmol) was dissolved in 10 mL of THF and cooled in a dry ice/acetone bath under nitrogen. Methylmagnesium bromide (1.33 mL, 4 mmol) was added via syringe over five mins. The reaction was stirred for 2 h at −70° C. DDQ (0.068g, 3 mmol) in 7 mL of THF was added and the mixture warmed to 25° C. The solvent was removed in vacuo and the residue was purified by silica gel chomatography using CH2Cl2 as the eluent to give compound 773A (0.15g, 42%) as a red oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07141578B2 |
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| 出典データセット | uspto-grants-2006_11 |
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| ORD ID | ord-3fb4bea0f53d44c4a058ee27d00617d4 |
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| 出典メモ | uspto-grants-2006_11 |
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