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N,N-dimethyl-5-nitropyridin-2-amine → N2,N2-dimethylpyridine-2,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-dimethyl-5-nitropyridin-2-amine | HCID 75707 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N2,N2-dimethylpyridine-2,5-diamine | HCID 78642 | 92% |
反応手順
A mixture of 0.312 g (1.87 mmol) of the above nitro compound and 0.205 g of 10% Pd/C in methanol (40 mL) was stirred under hydrogen (25 in/Hg) for 5 hrs. The reaction mixture was filtered through celite, and the solvent was concentrated, to give 0.236 g (92% yield) of N2,N2-dimethyl-2,5-pyridinediamine: 1H NMR (CDCl3) δ7.78 (d, J=2.9 Hz, 1H), 6.98 (dd, J=8.8, 2.9 Hz, 1H), 6.45 (dd, J=8.8, 0.5 Hz, 1H), 2.99 (s, 6H); LCMS (APCI+) m/z: 138 (MH+, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08486939B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-15192473680a4141831ad8eeab478da1 |
| 出典メモ | uspto-grants-2013_07 |