Sodium Iodide → HCID 10894686, Verbindung

HRID 1289398Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1289398
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[I-:22].[Na+]>CC(C)=O>[I:22][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

Komponenten

4

Edukt 2

HCID 5238Sodium IodideHCID 11100339Benzene, [[(12-bromododecyl)oxy]methyl]-

Produkt 1

HCID 10894686HCID 10894686, VerbindungAusbeute 104,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

First, 12.4 g of 1-bromo-12-benzyloxydodecane, 6.3 g of sodium iodide, and 125 ml of acetone were placed in a 200 ml flask whose content was replaced with argon. Then, the mixture was stirred under reflux for 5 hours. An insoluble matter was filtered away and a filtrate was concentrated. Thereafter, ether was introduced into the residue. The ether layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1) to obtain 14.7 g of 1-iodo-12-benzyloxydodecane (Y: 100%). The compound thus obtained had a purity of 96.1% by GC.

Aufarbeitung

  1. temperatureunder reflux for 5 hours
  2. filtrationAn insoluble matter was filtered away
  3. concentrationa filtrate was concentrated
  4. additionThereafter, ether was introduced into the residue
  5. washThe ether layer was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThereafter, the solvent was distilled away
  8. customThe residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1)

Quellen und Nachweise

ORD-Eintrag
ord-2d31262407d24d73bd6ec31c13ba9723
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05750213

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