化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Hydroxide → 3-[4-Chloro-3-(trifluoromethyl)phenyl]prop-2-enenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| 反応物 | 4-Chloro-3-(trifluoromethyl)benzaldehyde | HCID 118642 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-[4-Chloro-3-(trifluoromethyl)phenyl]prop-2-enenitrile | HCID 54176226 | 87.1% |
反応手順
A solution consisting of 10.6 g (0.06 mol) of diethyl cyanomethylphosphonate and 12.5 g (0.06 mol) of 4-chloro-3-trifluoromethylbenzaldehyde in 65 ml of tetrahydrofuran is added dropwise to a suspension of 6.7 g (0.12 mol) of powdered potassium hydroxide in 185 ml of tetrahydrofuran. During this process, there is a slight evolution of heat. Subsequently, the mixture is stirred at room temperature for 20 minutes and the solid material which separates off is filtered off and washed with tetrahydrofuran. The filtrate is concentrated in vacuo and the remaining residue is dried. 12.1 g (87.0% of theory) of 4-chloro-3-trifluoromethyl-cinnamonitrile are obtained as an E/Z isomeric mixture.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05428049 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-d4caff9d09254cf9a804c28ae2cf88db |
| 出典メモ | uspto-grants-1995_06 |