関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrite | HCID 946 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3,4-Bis(trifluoromethyl)aniline | HCID 1548579 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 触媒 | Nickel Sulfate | HCID 24586 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,4-Bistrifluoromethylbenzonitrile | HCID 14793271 | 63% |
反応手順
229 g (1 mole) of 3,4-bistrifluoromethyl-aniline were diazotized in a solution of 350 g of concentrated sulphuric acid in 1.25 1 of water using 70 g of sodium nitrite in 140 ml of water. After the diazonium salt solution had become nitrite-free, it was added dropwise to a solution of 550 ml of water, 210 g of sodium cyanide, 10 g of copper (I) cyanide, 500 g of sodium hydrogen carbonate and 9 g of nickel sulphate ×7 H2O heated to 100° C. The product was isolated from the reaction mixture by steam distillation and subsequently distilled again. 152 g of product having a boiling point at 14 mbar of 85° C. and a melting point of 71° to 72° C. were obtained. This corresponds to a yield of 63% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05142092 |
|---|
| 出典データセット | uspto-grants-1992_08 |
|---|
| ORD ID | ord-0c4b417b96ef4ab5af5fca5c67cd6ce8 |
|---|
| 出典メモ | uspto-grants-1992_08 |
|---|
