化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-(2-Amino-5-chloro-phenyl)-5-bromo-2-fluoro-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Chloro-1,2-diaminobenzene | HCID 7263 | — |
| 反応物 | 5-Bromo-2-fluorobenzoic acid | HCID 2736315 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-Amino-5-chloro-phenyl)-5-bromo-2-fluoro-benzamide | HCID 24699699 | 52% |
反応手順
Method 7—Step a A mixture of 5-Bromo-2-fluoro-benzoic acid (3.00 g, 13.70 mmol), 4-chloro-benzene-1,2-diamine (2.42 g, 16.99 mmol), HATU (5.47 g, 14.38 mmol) and TEA (1.91 mL, 13.83 mmol) in dichloromethane (70 mL) and DMF (16 mL) was stirred at room temperature overnight, then water was added (80 mL) and left standing at room temperature overnight. The organic layer was divided and solvent removed under reduced pressure and the crude oil obtained was crystallized from the mixture of solvents dichloromethane:cyclohexane/3:1 (30 mL) to afford 2.19 g of the title compound (52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835648B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b4ce010ef34c425eb8d782dbd571233d |
| 出典メモ | uspto-grants-2014_09 |