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1-Hydroxybenzotriazole → 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Benzo-1,3-dioxole-5-methylamine | HCID 75799 | — |
| 反応物 | 2-Fluoro-5-nitrobenzoic acid | HCID 280997 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide | HCID 22467641 | 86.1% |
反応手順
A mixture of 2-fluoro-5-nitrobenzoic acid (1.00 g), (1,3-benzodioxol-5-ylmethyl)amine (980 mg), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (1.55 g) and 1-hydroxybenzotriazole (1.09 g) in anhydrous dimethylformamide (10 mL) was stirred for 40 hours at ambient temperature. The mixture was partitioned between water and ethyl acetate. The separated organic layer was washed with an aqueous saturated sodium bicarbonate solution, 1N-hydrochloric acid, water and brine. Then, the resultant was dried over magnesium sulfate and evaporated in vacuo. The residue was triturated with diisopropyl ether to give 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide as yellow powders (1.48 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06384080B1 |
| 出典データセット | uspto-grants-2002_05 |
| ORD ID | ord-829a96a6ccff41a995f08c54de850f1f |
| 出典メモ | uspto-grants-2002_05 |