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Nitrogen → 5-(4-Amino-pyrazol-1-ylmethyl)-furan-2-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Methyl 5-[(4-nitro-1h-pyrazol-1-yl)methyl]-2-furoate | HCID 3157344 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-(4-Amino-pyrazol-1-ylmethyl)-furan-2-carboxylic acid methyl ester | HCID 66928890 | — |
反応手順
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 5-(4-nitro-pyrazol-1-ylmethyl)-furan-2-carboxylic acid methyl ester (4.45 g, 17.7 mmol) in MeOH (100 mL) was treated with Pd/C (445 mg, 10% Pd). The N2 atmosphere was replaced by an H2 atmosphere (H2 balloon) and the reaction mixture was stirred at rt for 4 h before being filtered through Celite and the solvent was removed under reduced pressure to give the title compound as an oil. LC-MS-conditions 02: tR=0.50 min; [M+H]+=222.27. 1H NMR (400 MHz, DMSO-d6) 1H NMR 83.79 (s, 3H), 3.88 (s, 2H), 5.24 (s, 2H), 6.54 (d, J=3.3 Hz, 1H), 6.96 (s, 1H), 7.08 (s, 1H), 7.25 (d, J=3.5 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08288419B2 |
| 出典データセット | uspto-grants-2012_10 |
| ORD ID | ord-3a71f2c655704c1ab41934c0d79ef3f7 |
| 出典メモ | uspto-grants-2012_10 |