Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Fluorobenzene → 2-Chloro-4-(4-fluorobenzoyl)-pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Fluorobenzene | HCID 10008 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Chloropyridine-4-carbonyl chloride | HCID 2800003 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Chloro-4-(4-fluorobenzoyl)-pyridine | HCID 20145710 | — |
반응 단계
To a solution of 4.2 g 2-chloro-isonicotinoyl chloride in 25 ml. fluorobenzene there is added with cooling 11.7 g AlCl3. The mixture is heated at 70°-80° C. during 7 hrs. The crude is added to acidic (pH 1-2) cold water. The pH is raised until 4.5 with diluted aqueous NaOH. This aqueous organic mixture is extracted several times with methylene chloride. The combined extracts are washed with water, dried (Na2SO4) and distilled in a rotary evaporator. The remaining crude oil is purified through a silica column, eluting with ethyl ether: petroleum ether 1:3. Yield 5 g of the title product, m.p. 60°-3° C. (cyclohexane); UV (ethanol) λmax.: 262 nm, ε=10,250; Cl 15.30 (15.05); F 8.15 (8.06).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04614833 |
| 출처 데이터셋 | uspto-grants-1986_09 |
| ORD ID | ord-fb11e132fb8a4f8c9668830b3e593a9f |
| 출처 메모 | uspto-grants-1986_09 |