化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2,2-Dimethyl-n-[3-(trifluoromethyl)phenyl]propanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-(Trifluoromethyl)aniline | HCID 7375 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2,2-Dimethyl-n-[3-(trifluoromethyl)phenyl]propanamide | HCID 714339 | 98.3% |
反応手順
A solution of pivaloyl chloride (3.62 g; 30 mmol) in 40 ml dry ether was added dropwise at room temperature to a mixture of 3-trifluoromethyl-aniline (4.83 g, 30 mmol) and triethylamine (4.25 ml, 30.5 mmol). This was stirred at room temperature for a period of 14 hours and then poured into 200 ml water, extracted with ether (2×100 ml). The combined ether extracts were washed successively with 0.5 HCl (100 ml); water (2×50 ml); 7% KOH (100 ml) and water (2×50 ml). The ether solution was dried with MgSO4 and concentrated in vacuo to give a white solid (7.23 gm, 98%, m.p. 112.5° C.). The 2,2-dimethyl-3'-trifluoromethyl-propionanilide was recrystallized with dichloromethane and petroleum ether mixture.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05248781 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-6cab89fbffc94bf8aa8d99d718c666ee |
| 出典メモ | uspto-grants-1993_09 |