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3-Methoxy-2-nitropyridine → 2-Amino-3-methoxypyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methoxy-2-nitropyridine | HCID 556063 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Amino-3-methoxypyridine | HCID 9920384 | 100% |
反応手順
To a solution of 2-nitro-3-methoxypyridine (32 g, 208 mmol) in EtOAc (150 mL) and MeOH (35 mL) under a nitrogen atmosphere was added 10% palladium on carbon (1.5 g, 1.4 mmol). This mixture was purged with H2 three times and the mixture was stirred for 3 h under a hydrogen atmosphere. The reaction mixture was purged with N2 three times, filtered through Celite, and the filter cake was washed with EtOAc (2×35 ml). The combined filtrate were concentrated and dried over high vacuum to afford 25.8 grams (100%) of 2-amino-3-methoxypyridine: LCMS (m/z): 125.0 (MH+); 1H NMR (300 MHz, CDCl3): 7.66 (m, 1H), 6.90 (m, 1H), 6.61 (m, 2H), 4.64 (s, br, 2H), 3.83 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865732B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-4978bc5377fc48e1b3f2b57e63efd495 |
| 出典メモ | uspto-grants-2014_10 |