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2,4,5-Trichloroaniline → 2,4,4',5,5'-Pentachloro-2'-methoxy-1,1'-biphenyl

HRID 1885517
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HRID 1885517 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([O:9][CH3:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[Cl:11][C:12]1[CH:18]=[C:17]([Cl:19])[C:16]([Cl:20])=[CH:15][C:13]=1N>>[CH3:10][O:9][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([Cl:8])=[CH:6][C:5]=1[C:13]1[CH:15]=[C:16]([Cl:20])[C:17]([Cl:19])=[CH:18][C:12]=1[Cl:11].[CH3:10][O:9][C:4]1[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[C:3]=1[C:13]1[CH:15]=[C:16]([Cl:20])[C:17]([Cl:19])=[CH:18][C:12]=1[Cl:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 124872,4,5-TrichloroanilineHCID 374381,2-Dichloro-4-methoxybenzene

생성물 2

HCID 198789142,4,4',5,5'-Pentachloro-2'-methoxy-1,1'-biphenylHCID 19878939HCID 19878939, 화합물

실험 절차

2-Methoxy-2',4,4',5,5'-pentachlorobiphenyl was prepared from 3,4-Dichloroanisole (35 g, 200 mmol) and 2,4,5-trichloroaniline (2.95 g, 15 mmol) according to the procedure in Example 2A. The excess dichloroanisole was removed by distillation and the residue was then filtered through silica gel (heptane eluent) and further purified [Chromatotron®, 4 mm silica gel, cyclohexane, 20 mL/min] to give 2-methoxy-2',4,4',5,5'-pentachlorobiphenyl (700 mg) and 2-Methoxy-2',4',5,5',6-pentachlorobiphenyl (1.2 g). Mass spectrum: m/z at 354 for C13H7Cl5O.

후처리

  1. customThe excess dichloroanisole was removed by distillation
  2. filtrationthe residue was then filtered through silica gel (heptane eluent)
  3. customfurther purified [Chromatotron®, 4 mm silica gel, cyclohexane, 20 mL/min]

출처 및 근거

ORD 기록
ord-42bc2d9eaec54b2180731eb9dc9e82dc
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05145790

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