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Sodium Carbonate → 6-(3-Phenyl-4-methoxyphenyl)-2-naphthaldehyde

HRID 860551
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HRID 860551 반응식
[C:1]1([C:7]2[CH:8]=[C:9](B(O)O)[CH:10]=[CH:11][C:12]=2[O:13][CH3:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[CH:25]=[C:24]([CH:29]=[O:30])[CH:23]=[CH:22]2.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.O.C(OCC)(=O)C.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[C:1]1([C:7]2[CH:8]=[C:9]([C:19]3[CH:20]=[C:21]4[C:26](=[CH:27][CH:28]=3)[CH:25]=[C:24]([CH:29]=[O:30])[CH:23]=[CH:22]4)[CH:10]=[CH:11][C:12]=2[O:13][CH3:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 10340Sodium CarbonateHCID 134770296-Bromonaphthalene-2-carbaldehydeHCID 21037383(4-Methoxy-3-phenylphenyl)boronic acid

생성물 1

HCID 865860406-(3-Phenyl-4-methoxyphenyl)-2-naphthaldehyde수율 86.9%

시약·촉매·용매 4

HCID 11979704Tetrakis(triphenylphosphine)palladium촉매
HCID 962
Water
용매
HCID 8857Ethyl Acetate용매
HCID 21863594Toluene ethanol용매

실험 절차

A mixture of 3-phenyl-4-methoxyphenyl boronic acid (0.465 g, 2.04 mmol), 6-bromo-2-naphthaldehyde (0.400 g, 1.70 mmol) and sodium carbonate (0.541 g, 5.10 mmol) in 10 mL of toluene:ethanol (4:1) and water (1 mL) was degassed with argon for 30 minutes. Tetrakis(triphenylphosphine) palladium(0) (0.059 g, 0.05 mmol) was added and the mixture heated at reflux for 17 hours. The solution was cooled to room temperature, diluted with ethyl acetate and washed successively with water and brine, dried over anhydrous magnesium sulfate, filtered and evaporated. The residue was purified on silica gel (eluent: hexane:EtOAc, 9:1) to give 0.50 g of 6-(3-phenyl-4-methoxyphenyl)-2-naphthaldehyde (86%) as a solid. 1H NMR (300 MHz; DMSO-d6, 300 MHz): δ 3.90 (s, 3H), 7.12 (d, J=9.0 Hz, 1H), 7.33–7.50 (m, 3H), 7.55-7.65 (m, 2H), 7.68–7.75 (m, 2H), 7.87 (dd, J1=8.4 Hz, J2=1.8 Hz, 1H), 7.97 (brs, 2H), 8.06 (d, J=9.0 Hz, 1H), 8.09 (d, J=1.0 Hz, 1H), 8.35 (s, 1H), 10.16 (s, 1H).

후처리

  1. customwas degassed with argon for 30 minutes
  2. temperaturethe mixture heated
  3. temperatureat reflux for 17 hours
  4. washwashed successively with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was purified on silica gel (eluent: hexane:EtOAc, 9:1)

출처 및 근거

ORD 기록
ord-dc4bf5aa10404bcba510fa2354abd673
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153875B2

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