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Water → 3,4-Difluoro-1-(2-methoxyethoxy)benzene

HRID 1968591
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HRID 1968591 반응식
[F:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[F:8].C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:16][O:17][CH2:18][CH2:19]Br.O>CN(C)C=O>[F:1][C:2]1[CH:3]=[C:4]([O:9][CH2:19][CH2:18][O:17][CH3:16])[CH:5]=[CH:6][C:7]=1[F:8]
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참가 물질

6

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 759273,4-DifluorophenolHCID 809722-Bromoethyl methyl ether

생성물 1

HCID 574290663,4-Difluoro-1-(2-methoxyethoxy)benzene수율 86.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 3,4-difluorophenol (2 g) and cesium carbonate (7.51 g) in N,N-dimethylformamide (15 mL) was added 2-methoxyethyl bromide (2.14 g), and the mixture was stirred at room temperature overnight. The reaction mixture was poured into water, and the resulting mixture was extracted with diethyl ether. The extract was washed with water twice and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=5/1) to give 3,4-difluoro-1-(2-methoxyethoxy)-benzene (2.49 g). To the solution of the obtained 3,4-difluoro-1-(2-methoxyethoxy)benzene (1.47 g) in tetrahydrofuran (39 mL) was added n-butyllithium (2.64 mol/L n-hexane solution, 3.25 mL) at −78° C., and the mixture was stirred at the same temperature for 30 minutes. To the reaction mixture was added dry ice (10 g), and the mixture was stirred at the same temperature for 30 minutes, and then stirred at room temperature for 30 minutes. To the reaction mixture was added 2 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (1.48 g).

후처리

  1. extractionthe resulting mixture was extracted with diethyl ether
  2. washThe extract was washed with water twice
  3. dry with materialbrine, and dried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=5/1)

출처 및 근거

ORD 기록
ord-2762452352a245e5939620f70c55b168
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426427B2

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