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Tetrahydrofuran → 9,10-Bis(4-heptyl)phenyl-2,6-dihydroxyanthracene

HRID 1166023
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1166023
[Si](O[C:9]1[CH:22]=[CH:21][C:20]2[C:19](=O)[C:18]3[C:13](=[CH:14][CH:15]=[C:16]([O:24][Si](C(C)(C)C)(C)C)[CH:17]=3)C(=O)[C:11]=2[CH:10]=1)(C(C)(C)C)(C)C.[Li][CH2:34][CH2:35][CH2:36][CH3:37].BrC1C=CC([CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH3:51])=CC=1.I.[CH2:53]1[CH2:57][O:56][CH2:55][CH2:54]1>>[CH3:37][CH2:36][CH2:35][CH:34]([C:17]1[C:10]2[C:53]([C:57]([CH:48]([CH2:47][CH2:46][CH3:45])[CH2:49][CH2:50][CH3:51])=[C:13]3[C:18]=1[C:19]([C:20]1[CH:11]=[CH:10][CH:9]=[CH:22][CH:21]=1)=[C:16]([OH:24])[CH:15]=[CH:14]3)=[CH:54][C:55]([OH:56])=[CH:22][CH:9]=2)[CH2:14][CH2:13][CH3:18]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 8028Tetrahydrofuran2×HCID 24841Hydrogen iodideHCID 27751001-Bromo-4-heptylbenzeneHCID 225907682,6-Bis(t-butyldimethylsilyloxy)anthraquinoneHCID 178418339Butyllithium

Produkt 1

HCID 880659029,10-Bis(4-heptyl)phenyl-2,6-dihydroxyanthracene
Ausbeute 51 %

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

Compound 2 (37 g, 0.079 mol) was dissolved in 200 mL of anhydrous THF and cooled to −78° C. To this solution was added n-BuLi (2.5 M in hexane, 94 mL, 0.24 mol) slowly to maintain the temperature below −60° C. After addition, the orange-yellow solution was stirred at −78° C. for an hour. Compound 1 (60.2 g, 0.24 mol) was dissolved in 100 mL of anhydrous THF and added dropwise to the above cooled solution. The reaction was slowly warmed up to room temperature and stirred at room temperature overnight. The reaction was quenched with HI aqueous solution (47% in water, 143 mL, 0.79 mol) and TBDMS group was also de-protected. The deep brown reaction was heated to reflux for 10 min. and most of the solvent was removed under reduced pressure. The reaction mixture was then extracted with methylene chloride three times. The combined organic phase was washed with saturated sodium metabisulfate solution, water, and brine, and dried over MgSO4. The crude product was obtained as brown viscous oil and was purified by column chromatography on silica gel with 10/90 ether/hexane as an eluent. The pure product was obtained as 22.4 g light yellow brown solid at 51% yield. 1H NMR (CDCl3) δ (ppm): 0.91 (t, J=7.0 Hz, 6H), 1.26-1.43 (m, 8H), 1.71-1.81 (m, 2H), 2.73 (t, J=7.8 Hz, 2H), 5.21 (s, br, 2H, OH), 6.89 (d, J=2.3 Hz, 2H), 6.96 (dd, J1=9.5 Hz, J2=2.5 Hz, 2H), 7.32 (d, J=8.6 Hz, 4H, phenyl), 7.35 (d, J=8.6 Hz, 4H, phenyl), 7.57 (d, J=9.4 Hz, 2H). 13C NMR (CDCl3): 14.16, 22.72, 29.26, 29.52, 31.60, 31.86, 35.90, 106.84, 118.58, 127.07, 128.46, 128.98, 129.64, 131.04, 134.94, 136.30, 142.10, 151.69. Mp 162-164° C. FD-MS: m/z 558 (M+).

Aufarbeitung

  1. temperatureto maintain the temperature below −60° C
  2. additionAfter addition
  3. additionadded dropwise to the above cooled solution
  4. temperatureThe reaction was slowly warmed up to room temperature
  5. stirringstirred at room temperature overnight
  6. customThe deep brown reaction
  7. temperaturewas heated
  8. temperatureto reflux for 10 min. and most of the solvent
  9. customwas removed under reduced pressure
  10. extractionThe reaction mixture was then extracted with methylene chloride three times
  11. washThe combined organic phase was washed with saturated sodium metabisulfate solution, water, and brine
  12. dry with materialdried over MgSO4
  13. customThe crude product was obtained as brown viscous oil
  14. customwas purified by column chromatography on silica gel with 10/90 ether/hexane as an eluent

Quellen und Nachweise

ORD-Eintrag
ord-740eb69103384c17adc4b79b37e1d4b0
Quelldatensatz
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06613457B2

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