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Dimethylformamide → 2-(Nitrophenyl)amino-3,4-dimethylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Nitroaniline | HCID 6946 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Iodo-3,4-dimethylbenzoic acid | HCID 11196635 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Nitrophenyl)amino-3,4-dimethylbenzoic acid | HCID 22742448 | 24.1% |
反応手順
10 g of 3,4-dimethyl-2-iodobenzoic acid, 6 g of 2-nitroaniline, 250 mg of powdery copper and 25 g of potassium carbonate were added to N,N-dimethylformamide and heated under reflux while stirring for 2 hr. Then the reaction mixture was cooled to room temperature and diluted with water. After adjusting the pH value thereof to pH 4 with conc. hydrochloric acid, it was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. After evaporating the solvent under reduced pressure, the residue was purified by silica gel column chromatography to give 2.5 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06703388B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-25156da413f74e3fb251e988748786fe |
| 出典メモ | uspto-grants-2004_03 |