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Formic Acid → 2,4-Dimethyl-3-nitroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | 1,3-Dimethyl-2,4-dinitrobenzene | HCID 69042 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,4-Dimethyl-3-nitroaniline | HCID 13369963 | — |
反応手順
A mixture of 2,6-dinitro-m-xylene (11.2 g) and 10% palladium on charcoal (620 mg) was stirred in triethylamine (36 mL) under an atmosphere of nitrogen and heated to reflux. Formic acid (9.25 mL) was added dropwise to the above mixture with vigorous stirring. After addition, the mixture was allowed to stir at reflux for an additional 15 min, then cooled to room temperature. The reaction mixture was diluted with ethyl acetate (100 mL) and filtered through celite. The filtrate was washed with brine and dried over magnesium sulfate. Evaporation afforded 9.51 g as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05952362 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-199164fec0c348ee973ed100368e6c4a |
| 出典メモ | uspto-grants-1999_09 |