関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Dihexylamine | HCID 8920 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Fluoro-5-nitrobenzonitrile | HCID 519417 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-cyano-N,N-dihexyl-4-nitroaniline | HCID 90022772 | 87.4% |
反応手順
To a solution of 2-fluoro-5-nitrobenzonitrile (1.83 g, 10.0 mmol) in CH3CN (20 mL) were added K2CO3 (2.76 g, 20.0 mmol) and dihexylamine (1.85 g, 9.98 mmol) and the mixture was stirred at 80° C. for 40 h. The mixture was cooled to rt, poured into 100 mL of DCM and washed with water (100 mL×3), brine (100 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=125:2) to give the title compound as yellow oil (2.89 g, 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434695B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-df9fc0513de84a9c85d6d8fc5a69e95c |
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| 出典メモ | uspto-grants-2016_09 |
|---|
