化工社化工社 化学情報印刷レポート · 研究参考用
1-Hydroxybenzotriazole → 5-amino-2,4-difluoro-N-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 5-Amino-2,4-difluorobenzoic acid | HCID 21049431 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-amino-2,4-difluoro-N-methylbenzamide | HCID 22019130 | 77.6% |
反応手順
5-amino-2,4-difluoro-benzoic acid (6 g, 34.6 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (13.3 g, 69.3 mmol) and 1-hydroxybenzotriazole (9.3 g, 69.3 mmol) was stirred in THF (100 ml). Diisopropylethylamine (7.2 ml, 41.5 mmol) and methylhydroxyamine hydrochloride (4.3 g, 51.9 mmol) were added thereto, and the solution was stirred for 5 hours. The resulting solution was extracted with ethylacetate and washed with salt solution. The resulting residue was recrystallized with diethylether to obtain the title compound 5 g (yield: 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846699B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-521e82beb46b4d0d8f1480c4ab46e1cd |
| 出典メモ | uspto-grants-2014_09 |