化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylamine → 2-chloro-4,5-difluoro-N,N-dimethylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Chloro-N,N-2-trimethylpropenylamine | HCID 640792 | — |
| 反応物 | 2-Chloro-4,5-difluorobenzoic acid | HCID 737171 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-chloro-4,5-difluoro-N,N-dimethylbenzamide | HCID 59346904 | 96.8% |
反応手順
A solution of 2-chloro-4,5-difluorobenzoic acid (385 mg, 2.0 mmol) in DCM (5 mL) was treated with (1-chloro-2-methylprop-1-en-1-yl)dimethylamine (293 mg, 2.2 mmol) and stirred under argon for 1 hour. The mixture was then treated with triethylamine (0.56 mL, 4.0 mmol) and a 2M solution of dimethylamine in THF (1.2 mL, 2.4 mmol), and stirred for 18 hours. The mixture was diluted with DCM (5 mL) and 2M hydrochloric acid (4 mL) and separated. The organic layer was dried (MgSO4), filtered and concentrated in vacuo to afford the title compound (425 mg). The residue was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745475B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-29d4985e8b5643428721490fac721520 |
| 出典メモ | uspto-grants-2010_06 |