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Methyl iodide → 1-Methyl-1h-indazole-3-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1H-Indazole-3-carbonitrile | HCID 437556 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Methyl-1h-indazole-3-carbonitrile | HCID 284700 | — |
反応手順
Sodium hydride (0.37 g, 60% dispersion in mineral oil) was added to a solution of 3-cyano-1H-indazole (1.20 g, Reference Example 57) in dry dimethylformamide (30 mL) under a nitrogen atmosphere at ambient temperature. The mixture was allowed to stir for 1 hour then treated with methyl iodide (0.85 mL) and stirring was continued for 1 hour. The reaction mixture was then poured into ice-water (15 mL). The precipitated solid was filtered then washed with water and then dried to give the title compound (0.80 g) as a beige solid, m.p. 73° C. 1H NMR [(CD3)2SO]: δ 7.91 (m, 2H); 7.60 (t, 1H); 7.42 (t, 1H); 4.21 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07943616B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-36ea6e95feea47b093279056759e9ad9 |
| 出典メモ | uspto-grants-2011_05 |