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Anisole → 3,4-Dichloro-4'-methoxybenzophenone

HRID 1857191
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HRID 1857191 반응식
[C:1]1([O:7][CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:9][C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][C:18]=1[Cl:19])[C:13](Cl)=[O:14].FC(F)(F)S([O-])(=O)=O.[Yb+3].FC(F)(F)S([O-])(=O)=O.FC(F)(F)S([O-])(=O)=O>[N+](C)([O-])=O>[CH3:8][O:7][C:1]1[CH:6]=[CH:5][C:4]([C:13]([C:12]2[CH:16]=[CH:17][C:18]([Cl:19])=[C:10]([Cl:9])[CH:11]=2)=[O:14])=[CH:3][CH:2]=1
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참가 물질

5

반응물 3

HCID 7519AnisoleHCID 76403Benzoyl chloride, 3,4-dichloro-HCID 2733225Ytterbium triflate

생성물 1

HCID 27581233,4-Dichloro-4'-methoxybenzophenone수율 10%

시약·촉매·용매 1

HCID 6375Nitromethane용매

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온도
60 °C

실험 절차

To commercially available nitromethane (10 ml) were added commercially available anisole (1.081 g), commercially available 3,4-dichlorobenzoyl chloride (2.095 g) and commercially available ytterbium(III) trifluoromethanesulfonate (620 mg), and the admixture was stirred at 60° C. for 8 hours. The reaction mixture was partitioned between water and chloroform, and the chloroform layer was then dried with anhydrous magnesium sulfate. After removing the solvent by reduced-pressure distillation, the resulting residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate to obtain 270 mg of the title compound (yield: 10%).

후처리

  1. customThe reaction mixture was partitioned between water and chloroform
  2. dry with materialthe chloroform layer was then dried with anhydrous magnesium sulfate
  3. customAfter removing the solvent
  4. distillationby reduced-pressure distillation
  5. customthe resulting residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-873b20d8028e43e3be8e2dcc019cc66d
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06143764

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