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4-Chloro-2-nitrophenol → 2,6-Bis(5-chloro-2-hydroxy-3-nitrobenzyl)-4-chlorophenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-2-nitrophenol | HCID 6980 | — |
| 反応物 | 4-Chloro-2,6-bis(chloromethyl)phenol | HCID 241197 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | 2,6-Bis(5-chloro-2-hydroxy-3-nitrobenzyl)-4-chlorophenol | HCID 13064214 | 18.8% |
反応手順
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°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04282390 |
| 出典データセット | uspto-grants-1981_08 |
| ORD ID | ord-281e04f5322b4fdb92f1fec382e91f1e |
| 出典メモ | uspto-grants-1981_08 |