化工社化工社 化学情報印刷レポート · 研究参考用
Water → 4-bromo-3-chloro-N-trimethylsilanylmethyl-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-(Trimethylsilyl)methylamine | HCID 87488 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 4-Bromo-3-chlorobenzoic acid | HCID 12594302 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-bromo-3-chloro-N-trimethylsilanylmethyl-benzamide | HCID 66836699 | — |
反応手順
To a solution of 4-bromo-3-chloro-benzoic acid (commercially available) (5.0 g) in dichloromethane (30 ml) was added N-(−3-dimethylaminopropyl)-N′-ethylcarbodiimid hydrochloride (5.29 g), N,N-dimethylaminopyridine (1.19 g) and trimethylsilylmethylamine (2.85 ml). The reaction mixture was stirred at ambient temperature for 5 hours. Water and dichloromethane was added to the reaction mixture. The phases were separated and the organic phase was washed with brine, dried over sodium sulfate and filtered through silica gel. The reaction mixture was concentrated to give 4-bromo-3-chloro-N-trimethylsilanylmethyl-benzamide (4.87 g). 1H-NMR (400 MHz, CDCl3): 7.68 (d, 1H), 7.55 (s, 1H), 7.33 (d, 1H), 5.85 (s, 1H), 2.84 (d, 2H), 0.00 (s, 9H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946447B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-a3c1a6b6daf04fb9b085f17a021f3c52 |
| 出典メモ | uspto-grants-2015_02 |