Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Chloro-2-nitrophenol → 2,6-Bis(5-chloro-2-hydroxy-3-nitrobenzyl)-4-chlorophenol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Chloro-2-nitrophenol | HCID 6980 | — |
| 반응물 | 4-Chloro-2,6-bis(chloromethyl)phenol | HCID 241197 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 생성물 | 2,6-Bis(5-chloro-2-hydroxy-3-nitrobenzyl)-4-chlorophenol | HCID 13064214 | 18.8% |
반응 단계
Zinc chloride (2 g) was added in small portions over 75 min to a melt of 2,6-bis(chloromethyl)-4-chlorophenol (1.2 g) and 4-chloro-2-nitrophenol (3 g) at a temperature of 120°. The mixture was stirred at this temperature for approximately 1 hr. The black product was extracted several times with acetone and the extract filtered to remove black inorganic material. The acetone was removed by distillation under reduced pressure and the residue chromatographed on silica gel. Elution with hexane containing 3% ethyl acetate gave unreacted 4-chloro-2-nitrophenol and elution with hexane containing 20% ethyl acetate gave the title compound (0.5 g) which was recrystallised from aqueous ethanol; m.p. 200°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04282390 |
| 출처 데이터셋 | uspto-grants-1981_08 |
| ORD ID | ord-281e04f5322b4fdb92f1fec382e91f1e |
| 출처 메모 | uspto-grants-1981_08 |