関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Fluoro-5-(trifluoromethyl)aniline | HCID 136349 | — |
| 反応物 | Potassium ethylxanthate | HCID 2735045 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Ethoxythiocarbonylthio-4-fluorobenzotrifluoride | HCID 12097353 | 99% |
反応手順
2-Fluoro-5-trifluoromethylaniline (14 g) was suspended in 30 ml of water and 10 ml of concentrated hydrochloric acid. The suspension was cooled to −5° C. while a solution of 5.93 g of sodium nitrite in 30 ml of water was added dropwise, followed by stirring at −59° C. for 2 hours. Then the solution was added to a solution of 16 g of potassium O-ethyl dithiocarbonate in 20 ml of water (40 to 50° C.), followed by stirring for 1 hour. The reaction mixture was extracted with an aqueous solution of ethyl acetate, dried and concentrated, giving 22 g of 3-ethoxythiocarbonylthio-4-fluorobenzotrifluoride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06710062B1 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-0f9fecd1643e4add9ad5763b945bc4a1 |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|