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3-Pyridinemethanamine → 3-Fluoro-4-nitro-N-(3-pyridylmethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Pyridinemethanamine | HCID 31018 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Fluoro-4-nitrobenzoic acid | HCID 230653 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 3-Fluoro-4-nitro-N-(3-pyridylmethyl)benzamide | HCID 59198667 | — |
反応手順
3-Fluoro-4-nitrobenzoic acid 2.78 g, 3-pyridylmethylamine 1.55 mL, N,N-diisopropylethylamine 2.61 mL, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride 4.31 g, 1-hydroxybenzotriazole monohydrate 2.98 g and acetonitrile 39 mL were mixed and stirred for 20 hours. The reaction liquid was poured in saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine by the order stated, and dried over magnesium sulfate. Distilling the solvent off, 4.09 g of the title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829000B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b2ee502842fb410a956edc914c523915 |
| 出典メモ | uspto-grants-2014_09 |