Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 2-Methyl-3,4,6-trifluorobenzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Potassium Cyanide | HCID 9032 | — |
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | 3,4,6-Trifluoro-2-methylaniline | HCID 22625178 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 촉매 | Copper Sulfate | HCID 24462 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Methyl-3,4,6-trifluorobenzonitrile | HCID 22625175 | 38.2% |
반응 단계
To 2-methyl-3,4,6-trifluoroaniline (10.6 g) is added a mixture of conc. sulfuric acid (13.8 ml) and water (46 ml) and the mixture is cooled. Thereto an aqueous solution (20 ml) of sodium nitrite (5.5 g) is added dropwise at 0°-5° C. The solution is gradually added to a mixture of copper (II) sulfate 5 hydrate (41 g), potassium cyanide (43 g), ammonium hydroxide (60 ml) and water (260 ml) at 10°-30° C. The mixture is extracted with dichloromethane and the extract is dried over sodium sulfate, concentrated and the residue is purified with column chromatography (silica-gel, dichloromethane:n-hexane=1:4) to give 2-methyl-3,4,6-trifluorobenzonitrile (4.3 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05723648 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-1e9ca78c8b7943d3b81ed784f0fbf2a2 |
| 출처 메모 | uspto-grants-1998_03 |