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Potassium Carbonate → 2-[2-(2,4'-Difluorobiphenyl-4-yl)ethyl]naphthalene

HRID 1712196
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HRID 1712196 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]2[CH:20]=[CH:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=2)[CH:5]=[CH:6][C:7]=1I.[F:21][C:22]1[CH:27]=[CH:26][C:25](OB(O)O)=[CH:24][CH:23]=1.C([O-])([O-])=O.[K+].[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1(C)C=CC=CC=1.O.C(O)C>[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]2[CH:20]=[CH:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=2)[CH:5]=[CH:6][C:7]=1[C:25]1[CH:26]=[CH:27][C:22]([F:21])=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 11776TriphenylphosphineHCID 219397714-Fluoro-phenylboric acidHCID 686151912-[2-(3-Fluoro-4-iodophenyl)ethyl]naphthalene

생성물 1

HCID 686169402-[2-(2,4'-Difluorobiphenyl-4-yl)ethyl]naphthalene

시약·촉매·용매 3

HCID 74236
Tetrabutylammonium Bromide
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 86587398Ethanol toluene water용매

실험 절차

A mixture of 7.00 g (=18.61 mmol) of the above 2-[2-(3-fluoro-4-iodophenyl)ethyl]naphthalene, 3.12 g (=22.30 mmol) of 4-fluorophenylboric acid, 3.86 g (=27.93 mmol) of K2CO3, 1.50 g (=4.65 mmol) of tetrabutylammonium bromide, 0.39 g (=0.56 mmol) of dichlorobis(triphenylphosphine)palladium(II), 0.30 g (1.12 mmol) of triphenylphosphine and 60 ml of a mixed solvent of toluene/water/ethanol in a ratio of 1:1:1 was stirred for 4 hours with reflux. The reaction mixture obtained was extracted thrice with toluene, and then the extract was washed thrice with water and dried with anhydrous MgSO4. After the solvent was evaporated under a reduced pressure, the obtained orange solid of 8.48 g was purified with silica gel chromatography using heptane/toluene in a ratio of 5:1 as the eluent to obtain a white solid of 7.37 g, which was further recrystallized using a mixed solvent of Solumix/heptane in a ratio of 1:1 to obtain the target compound in an amount of 5.02 g. The product was characterized as the target compound based on results of various instrumental analyses, and the phase transition of the product is notated as “C 108.1 I”.

후처리

  1. temperaturewith reflux
  2. customThe reaction mixture obtained
  3. extractionwas extracted thrice with toluene
  4. washthe extract was washed thrice with water
  5. dry with materialdried with anhydrous MgSO4
  6. customAfter the solvent was evaporated under a reduced pressure
  7. customthe obtained orange solid of 8.48 g was purified with silica gel chromatography
  8. customto obtain a white solid of 7.37 g, which
  9. customwas further recrystallized
  10. customto obtain the target compound in an amount of 5.02 g
  11. customon results of various instrumental analyses

출처 및 근거

ORD 기록
ord-a70c005585534082a5b23b7877cddb72
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790915B2

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