化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2-(4-Bromo-phenyl)-N-{4-[2-(4-bromo-phenyl)-2-hydroxy-acetylamino]-phenyl}-2-hydroxy-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | P-Phenylenediamine | HCID 7814 | — |
| 反応物 | p-Bromomandelic acid | HCID 97930 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 2-(4-Bromo-phenyl)-N-{4-[2-(4-bromo-phenyl)-2-hydroxy-acetylamino]-phenyl}-2-hydroxy-acetamide | HCID 68027740 | 95% |
反応手順
In a 250 cm3 flask fitted with a consender and a reverse Dean-Stark apparatus, the (4-bromo-phenyl)-hydroxy-acetic acid (25.00 g, 108.2 mmol) and 1,4-phenylenediamine (3.900 g, 36.07 mmol) are dissolved in chlorobenzene (100 cm3). The reaction mixture is heated to 132° C. while the generated water is distilled off the using the reverse Dean-Stark apparatus. After 21 hours, the reaction mixture is cooled down, the precipitate is filtered off and washed with methanol to yield the product (18.21 g, Yield: 95%). NMR (1H, 300 MHz, CDCl3): δ 9.90 (br, 2H); 7.59 (s, 4H); 7.56 (d, J=8.5 Hz, 4H); 7.45 (d, J=8.5 Hz, 4H); 6.53 (d, J=4.7 Hz, 2H), 5.08 (d, J=4.7 Hz, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09287504B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-9494d1c9e7034ca39eb730abbeb12e6a |
| 出典メモ | uspto-grants-2016_03 |