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Pyridine → 3-(2-Dimethylamino-ethoxy)-2'-methyl-biphenyl-4-carbaldehyde

HRID 30618
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 30618
[OH:1][C:2]1[CH:9]=[C:8](O)[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].N1C=CC=CC=1.FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.[C:32]1([CH3:41])[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].[H-].[Na+].[CH3:50][N:51]([CH3:55])[CH2:52][CH2:53]Cl>C(Cl)Cl.COCCOC.O.C1(C)C=CC=CC=1.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>[CH3:50][N:51]([CH3:55])[CH2:52][CH2:53][O:1][C:2]1[CH:9]=[C:8]([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=2[CH3:41])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

13

Edukt 7

HCID 1049PyridineHCID 72132,4-DihydroxybenzaldehydeHCID 79012-Chloro-N,N-dimethylethylamineHCID 10340Sodium CarbonateHCID 24758Sodium hydrideHCID 67749Trifluoromethanesulfonic anhydrideHCID 27332672-Methylphenyl boronic acid

Produkt 1

HCID 866010083-(2-Dimethylamino-ethoxy)-2'-methyl-biphenyl-4-carbaldehyde

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 178418476HCID 178418476, VerbindungKatalysatorHCID 962WaterLösungsmittelHCID 1140TolueneLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

A solution of 2,4-dihydroxybenzaldehyde (27 mmol) in methylene chloride (10 ml) and pyridine (30 mmol) was slowly added trifluoromethanesulfonic anhydride (32 mmol) keeping the temperature below 5° C. After 10 min the mixture was washed with water and the organic phase was concentrated under reduced pressure. The crude brown oil (5 g), ortho-tolylboronic acid (20.4 mmol), sodium carbonate (55.5 mmol) and dichlorobis(triphenylphosphine)-palladium (II) (3 mol %) was dissolved in DME (50 ml) and water (20 ml). The mixture was refluxed for 17 h under Argon, cooled to room temperature and extracted with ethyl acetate. The crude black oil (4.6 g) was dissolved in DMF (75 ml) and sodium hydride (60% in oil, 22.5 mmol) was slowly added. A solution of 2-dimethylamino ethylchloride (22.5 mmol) in toluene (120 ml) was added and the mixture was heated at 80° C. for 3 days. The mixture was washed with saturated sodium bicarbonate, concentrated under reduced pressure and purified by chromatography. The resulting yellow oil was washed with hot heptane giving the product as relative pure oil (GC-MS). 1H-NMR (DMSO-d6) δ 10.41 (s, 1H), 7.74 (d, 2H), 7.66-7.55 (m, 1H), 7.36-6.79 (m, 4H), 4.27 (t, 2H), 2.70 (t, 2H), 2.27 (s, 3H), 2.23 (s, 6H).

Aufarbeitung

  1. customthe temperature below 5° C
  2. washAfter 10 min the mixture was washed with water
  3. concentrationthe organic phase was concentrated under reduced pressure
  4. temperatureThe mixture was refluxed for 17 h under Argon
  5. extractionextracted with ethyl acetate
  6. dissolutionThe crude black oil (4.6 g) was dissolved in DMF (75 ml)
  7. temperaturethe mixture was heated at 80° C. for 3 days
  8. washThe mixture was washed with saturated sodium bicarbonate
  9. concentrationconcentrated under reduced pressure
  10. custompurified by chromatography
  11. washThe resulting yellow oil was washed with hot heptane giving the product as relative pure oil (GC-MS)

Quellen und Nachweise

ORD-Eintrag
ord-e9f887c92ce84f78af53796f22ec052b
Quelldatensatz
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07423181B2

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