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Ethyl Bromide → N,N-Diethyl-m-phenetidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Bromide | HCID 6332 | — |
| 反応物 | 3-(Diethylamino)phenol | HCID 7062 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | N,N-Diethyl-m-phenetidine | HCID 74625 | 91.1% |
反応手順
A 1 liter reactor is charged with 300 ml of methyl isobutyl ketone, 73.1 g of 3-diethylaminophenol and 153.3 g of ground potassium carbonate and the mixture is stirred for 30 minutes. Then 72.7 g of ethyl bromide are introduced into the autoclave, which is then closed and heated for 3 hours to 115°-120° C. The temperature is then kept for a further 5 hours at 140°-142° C. (pressure: 5 bar). The contents of the autoclave are cooled to c. 25° C. and potassium bromide is removed by filtration. After washing with a small amount of methyl isobutyl ketone, the combined filtrates are concentrated by evaporation, to give 75.6 g (91.1% yield) of 3-diethylaminophenetol with a titre of 96.9%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04825005 |
| 出典データセット | uspto-grants-1989_04 |
| ORD ID | ord-f5e0d1425a7d4291b9e97b8afe455367 |
| 出典メモ | uspto-grants-1989_04 |