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Diisopropyl Ether → 1,2-Dichloro-3-(trifluoromethyl)-5-[1-(trifluoromethyl)ethenyl]benzene

HRID 551337
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HRID 551337 반응식
Br[C:2]1[CH:3]=[C:4]([Cl:13])[C:5]([Cl:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.C(OC(C)C)(C)C.C([Li])CCC.COB(OC)OC.Br[C:34]([C:36]([F:39])([F:38])[F:37])=[CH2:35].C(=O)([O-])[O-].[K+].[K+]>CCCCCC.O1CCCC1.CC(C1C=CC=C(C(C)C)C=1N1C(=[Pd])N(C2C(C(C)C)=CC=CC=2C(C)C)C=C1)C.CC(C1C=CC=C(C(C)C)C=1N1C(=[Pd])N(C2C(C(C)C)=CC=CC=2C(C)C)C=C1)C.C1C=C2C(C(C=CC2=O)=O)=CC=1.C1C=C2C(C(C=CC2=O)=O)=CC=1.C(OCC)(=O)C.O>[Cl:13][C:4]1[CH:3]=[C:2]([C:34]([C:36]([F:39])([F:38])[F:37])=[CH2:35])[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[C:5]=1[Cl:12]
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참가 물질

12

반응물 6

HCID 7914Diisopropyl EtherHCID 8470Trimethyl borateHCID 11430Potassium CarbonateHCID 2726961-Propene, 2-bromo-3,3,3-trifluoro-HCID 250672915-Bromo-1,2-dichloro-3-(trifluoromethyl)benzeneHCID 178418339Butyllithium

생성물 1

HCID 86643384
1,2-Dichloro-3-(trifluoromethyl)-5-[1-(trifluoromethyl)ethenyl]benzene
수율 79.1%

시약·촉매·용매 5

HCID 111824871,3-Bis(2,6-diisopropylphenyl)imidazol-2-ylidene(1,4-naphthoquinone)palladium(0) dimer촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매2회HCID 8857Ethyl Acetate용매

실험 절차

To a stirred solution of 5-bromo-2,3-dichlorobenzotrifluoride (26.2 g) and diisopropyl ether (9.1 g) in hexane (250 mL) at −10° C. was added dropwise 1.55M n-butyllithium in hexane (57.5 mL). After stirring at same temperature for 0.5 hour, trimethoxyborane (9.26 g) in tetrahydrofuran (30 mL) was added dropwise. After a further 10 minutes, water (150 mL), 2-bromo-3,3,3-trifluoropropene (23.4 g), potassium carbonate (36.9 g) and 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene(1,4-naphthoquinone)palladium(0) dimer (0.131 g) were added to the reaction mixture, which was stirred at 60° C. for 4 hours. After the completion of the reaction, the reaction mixture was cooled to room temperature, poured into ice-water (50 mL) and ethyl acetate (75 mL) and filtered. The filtrate was separated, and the organic layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to provide a residue. The residue was purified by column chromatography on silica gel eluted with hexane to afford the title compound as a colorless oil (21.8 g).

후처리

  1. waitAfter a further 10 minutes
  2. stirringwas stirred at 60° C. for 4 hours
  3. customAfter the completion of the reaction
  4. filtrationfiltered
  5. customThe filtrate was separated
  6. washthe organic layer was washed with water and brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customto provide a residue
  10. customThe residue was purified by column chromatography on silica gel
  11. washeluted with hexane

출처 및 근거

ORD 기록
ord-327dc3a49abf4c7fa07fb35a6e91f93d
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07947715B2

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