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Hydrazine → 2,4-Dimethoxybenzohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | Benzoic acid, 2,4-dimethoxy-, methyl ester | HCID 137451 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,4-Dimethoxybenzohydrazide | HCID 456728 | 78.1% |
反応手順
Ex-109A: A solution of 2,4-dimethoxy-benzoic acid methyl ester (4.24 g, 21.6 mmol) and hydrazine (3.4 mL, 108.1 mmol) in methanol (50 mL) was refluxed overnight. Solvent was removed under reduced pressure. The residue was re-dissolved in ethyl acetate. The solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine, dried over sodium carbonate and concentrated to afford 2,4-dimethoxy-benzoic acid hydrazide (3.31 g, 78%) as a white solid: 1H NMR (CDCl3) δ 8.77 (bs, 1H), 8.15 (d, J=8.8 Hz, 1H), 6.58 (dd, J=8.8, 2.2 Hz, 1H), 6.46 (d, J=2.2 Hz, 1H), 4.10 (bs, 2H), 3.91 (s, 3H), 3.83 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094801B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-665a71c8df494a06987f1f3e49f3c7d1 |
| 出典メモ | uspto-grants-2006_08 |