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2-Amino-6-methyl-3-nitropyridine → 6-Methylpyridine-2,3-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-6-methyl-3-nitropyridine | HCID 226028 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Methylpyridine-2,3-diamine | HCID 2734420 | 96.5% |
反応手順
6-Methyl-3-nitro-pyridin-2-ylamine (1.3 g, 8.5 mmol) was dissolved in methanol (40 ml). The flask was purged of all oxygen, placed under a nitrogen atmosphere, and charged with Pd/C (150 mg of 10% palladium on carbon). The reaction mixture was purged, and placed under a hydrogen atmosphere, maintained with a balloon. It was allowed to stir for 18 h until the reduction was judged complete. It was then filtered through Celite™ to remove the palladium. The solvent was removed under vacuum to yield the title compound (1.01 g, 96%). 1H NMR (DMSO-d6): δ=6.59 (d, 1H, J=7.5 Hz), 6.19 (d, 1H, J=7.5 Hz), 5.23 (bs, 2H), 4.39 (bs, 2H), 2.11 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07696210B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-3d4f1e8890094c83b6291422c1739e3b |
| 出典メモ | uspto-grants-2010_04 |