3,4-Dichlorophenol → 2-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzene

HRID 1416347

반응식

HRID 1416347 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[Cl:8].Cl[C:11]1[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][C:12]=1[N+:21]([O-:23])=[O:22].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:21]([C:12]1[CH:13]=[C:14]([C:17]([F:18])([F:19])[F:20])[CH:15]=[CH:16][C:11]=1[O:9][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([Cl:8])=[CH:6][CH:5]=1)([O-:23])=[O:22]

참가 물질

5

반응물 3

HCID 72583,4-DichlorophenolHCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 11430Potassium Carbonate

생성물 1

HCID 13430092-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

A mixture of 3,4-dichlorophenol (25 gram (hereinafter g), 0.153 mol), 4-chloro-3-nitrobenzo-trifluoride (52 g, 0.23 mol) and potassium carbonate (63 g, 0.459 mol) in dimethylformamide (450 mL)was stirred under argon at 120° C. for 24 h. The reaction mixture was filtered and the filtrate evaporated. The residue was dissolved in ethyl acetate, washed with water, brine, dried over anhydrous magnesium sulfate, filtered and evaporated. The residue was flash chromatographed (silica gel, methylene chloride/hexane), to give the title compound as a yellow oil.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate evaporated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customchromatographed (silica gel, methylene chloride/hexane)

출처 및 근거

ORD 기록
ord-758458e104394928a7c4f28ffe609edd
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05912270

연결된 노트

불러오는 중…