関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Methyl 3-methoxy-4-nitrobenzoate | HCID 287308 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Methoxy-4-nitrobenzohydrazide | HCID 21883875 | 71% |
反応手順
To methyl 3-methoxy-4-nitrobenzoate (5.16 g, 24.5 mmol) in EtOH (250 mL) was added hydrazine monohydrate (5.95 mL, 122 mmol) in one portion. The reaction was heated at 80° C. overnight and concentrated upon completion by TLC. The residue was taken up in EtOAc, heated and hot filtered. The filtrate was concentrated and the residue was triturated with diethyl ether to provide the title compound (3.65 g, 17.3 mmol, 71%). 1H NMR (400 MHz, DMSO-d6) δ ppm 3.96 (s, 3H), 4.60 (br. s., 2H), 7.50 (dd, J=8.4, 1.5 Hz, 1H), 7.69 (d, J=1.8 Hz, 1H), 7.93 (d, J=8.1 Hz, 1H), 10.05 (br. s., 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08093239B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-8caec853cd82465a9d01bdaf8f8adf24 |
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| 出典メモ | uspto-grants-2012_01 |
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