関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1-Dibenzylhydrazine | HCID 197050 | — |
| 反応物 | 2-Amino-4,5-difluorobenzoic acid | HCID 735965 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Amino4,5-difluorobenzoic acid, 2,2-dibenzylhydrazide | HCID 86607132 | 157.5% |
反応手順
4,5-Difluoroanthranilic acid (4.73 g, 27.3 mmol) and N,N-dibenzylhydrazine (8.69 g, 42 mmol) are combined in 200 mL of methylene chloride. 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDAC) (7.85 g, 41 mmol) is then added to this solution, and the mixture is stirred for 18 hours at 25° C., The solution is washed with saturated NaHCO3, brine, and dried over magnesium sulfate. The solution is concentrated to give 15.8 g of a dark oil and purified via chromatography (SiO2, CHCl3) to give 3.4 g of the title compound as a solid. MS CI: m/z 368 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07094780B1 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-7f92a3d7fb874808929e1d951998575f |
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| 出典メモ | uspto-grants-2006_08 |
|---|
