関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4,5-Dichloro-2-nitroaniline | HCID 81149 | — |
| 反応物 | Piperazine-2-carboxylic acid | HCID 2723758 | — |
| 溶媒 | Cyclohexanol | HCID 7966 | — |
| 生成物 | 5-(3-Carboxypiperazin-1-yl)-4-chloro-2-nitroaniline | HCID 22272964 | 72.1% |
反応手順
To a solution of 2.10 g of 4,5-dichloro-2-nitroaniline and 2.20 g of 2-piperazinecarboxylic acid in 20 ml of cyclohexanol, 4.80 g of sodium carbonate was added, followed by 14 hours' stirring at 150° C. After cooling the reaction liquid to room temperature, water was added and the system was washed with chloroform. The aqueous layer was purified with an ion-exchange resin (Diaion HP-20, Mitsubishi Kasei, eluent: methanol). Upon condensing the fraction containing the object product under reduced pressure, 2.20 g of the title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06969712B2 |
|---|
| 出典データセット | uspto-grants-2005_11 |
|---|
| ORD ID | ord-5da0a42d4ec442708176b763c252be1f |
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| 出典メモ | uspto-grants-2005_11 |
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