Sodium Carbonate → HCID 16122316, 화합물

HRID 467415

반응식

HRID 467415 반응식
Br[C:2]1[CH:3]=[C:4]([O:8][CH3:9])[CH:5]=[CH:6][CH:7]=1.[C:10]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:11](B(O)O)=[CH:12][CH:13]=[CH:14][CH:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>COC>[CH3:9][O:8][C:4]1[CH:3]=[C:2]([C:24]2[C:19]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:7]=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 169713-BromoanisoleHCID 4589187Biphenyl-2-boronic acid

생성물 1

HCID 16122316HCID 16122316, 화합물수율 90%

시약·촉매·용매 1

HCID 8254Dimethyl Ether용매

실험 절차

Under an argon atmosphere, 18.7 g of 3-bromoanisole, 23.8 g of 2-biphenylboronic acid and 2.31 g of tetraxis(triphenylphosphine)palladium(0) were placed in a flask. 340 mL of dimethyl ether (DME) and 170 mL of a 2M aqueous sodium carbonate solution were added to this flask, and the resultant was refluxed with stirring while heating for 8 hours. After cooling to room temperature, an aqueous phase was removed. An organic phase was washed with water and saturated brine, and then dried with magnesium sulfate. After the magnesium sulfate was filtered out, the organic phase was concentrated. The resulting residue was purified by means of silica gel column chromatography, whereby 23.4 g (yield: 90%) of intended 3-methoxy[1,1′:2′,1″]terphenyl was obtained.

후처리

  1. temperaturethe resultant was refluxed
  2. temperaturewhile heating for 8 hours
  3. customan aqueous phase was removed
  4. washAn organic phase was washed with water and saturated brine
  5. dry with materialdried with magnesium sulfate
  6. filtrationAfter the magnesium sulfate was filtered out
  7. concentrationthe organic phase was concentrated
  8. customThe resulting residue was purified by means of silica gel column chromatography

출처 및 근거

ORD 기록
ord-89b77e8de0a0479085a03dbb5cf7c495
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623520B2

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