化工社化工社 化学情報印刷レポート · 研究参考用
Sulfuric Acid → Crotonic acid 2,2,2-trichloroethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | Trichloroethanol | HCID 8259 | — |
| 反応物 | Crotonic Acid | HCID 637090 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Crotonic acid 2,2,2-trichloroethyl ester | HCID 15703159 | 95% |
反応手順
In 200 ml. carbon tetrachloride are dissolved 0.5 mole (43.07 g.) crotonic acid and the equimolar amount of 2,2,2-trichloroethanol, 1 ml. concentrated sulphuric acid is added thereto and the reaction mixture is heated under reflux on a water separator until the theoretical amount of water (9 ml.) has separated off. Subsequently, the organic phase is shaken out twice with, in each case, 100 ml. aqueous 2N sodium hydrogen carbonate solution and twice with, in each case, 50 ml. of water, the organic phase is then dried with anhydrous magnesium sulphate and the solvent is distilled off in a vacuum. There is finally obtained the desired product (i) in the form of a bright yellow oil in a yield of 95% of theory. C6H7O2Cl3. (217.4791).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05214195 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-f50bdbb835e34209bf80adf5c63d8046 |
| 出典メモ | uspto-grants-1993_05 |