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Methyl 2-amino-4-chloro-5-nitrobenzoate → 4-Chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-5-nitro-benzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 2-amino-4-chloro-5-nitrobenzoate | HCID 15895692 | — |
| 反応物 | (3,5-Dimethylphenyl)acetyl chloride | HCID 15895699 | — |
| 生成物 | 4-Chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-5-nitro-benzoic acid methyl ester | HCID 54313456 | 72.4% |
反応手順
To a suspension of 2-amino-4-chloro-5-nitrobenzoic acid methyl ester (989 mg in 15 mL of dry 1,2-dichloroethane) was added a solution of (3,5-dimethylphenyl)acetyl chloride (860 mg in 5 mL dry 1,2-dichloroethane) and the mixture heated at reflux on an oil bath. After 18 hours, an additional portion of (3,5-dimethylphenyl)acetyl chloride (274 mg in 1.5 mL dry 1,2-dichloroethane) was added and the mixture heated at reflux for an additional 5 hours. At this time the reaction was cooled and the solvent removed in vacuo. Recrystallization of the crude product from methanol gave the title compound (1.17 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06150352 |
| 出典データセット | uspto-grants-2000_11 |
| ORD ID | ord-0a55e9c5fc4046499b7ad5b86da0edc5 |
| 出典メモ | uspto-grants-2000_11 |