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3-Fluoro-4-nitroaniline → Cyclohexyl-n-(3-fluoro-4-nitrophenyl)carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Fluoro-4-nitroaniline | HCID 75401 | — |
| 反応物 | Cyclohexanecarbonyl chloride | HCID 75938 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofurane dichloromethane | HCID 21919333 | — |
| 生成物 | Cyclohexyl-n-(3-fluoro-4-nitrophenyl)carboxamide | HCID 58742600 | 80.7% |
反応手順
3-Fluoro-4-Nitroaniline (1 mmol, 0.15 g) was dissolved in a 3:1 mixture of CH2Cl2/THF (4 mL) and pyridine (0.2 mL) was added to the mixture, which was cooled in an ice-water bath under nitrogen. Cyclohexanecarbonylchloride (1.1 mmol, 0.162 g) was dissolved in CH2Cl2 (1 mL) and added dropwise to the above solution at 4° C. and stirred at room temperature for 3 h. The reaction mixture was diluted with CH2Cl2 (50 mL) and washed with 1N HCl, 10% NaHCO3, brine and water, dried over Na2SO4 and the solvent evaporated to afford cyclohexyl-N-(3-fluoro-4-nitrophenyl)carboxamide (0.215 g) of product (Yield: 81%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07138420B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-742fac2e64c547abbb39b88fb01a7247 |
| 出典メモ | uspto-grants-2006_11 |