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Water → HCID 87088126, Verbindung

HRID 1053542
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1053542
[CH2:1]([OH:21])[CH2:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20].[C:22]([O:26]Br)(=[O:25])[CH2:23][CH3:24].[OH-].[Na+].O.[C:31]1([CH3:37])[CH:36]=CC=C[CH:32]=1>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:1]([O:21][CH:23]([CH3:24])[C:22]([O:26][C:31]([CH3:37])([CH3:36])[CH3:32])=[O:25])[CH2:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 962WaterHCID 1140TolueneHCID 14798Sodium HydroxideHCID 11228909Hypobromous acid, anhydride with propanoic acidHCID 59539494(5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol

Produkt 1

HCID 87088126HCID 87088126, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 70681Tetrabutylammonium ChlorideKatalysator

Versuchsvorschrift

A mixture of (5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol, (1.00 g, 3.47 mmol), tetrabutylammonium chloride (0.24 g, 0.87 mmol) and t-butyl □-bromo propionate (3.62 g, 17.3 mmol) was dissolved in toluene (36 mL) and placed under nitrogen. An aqueous solution of sodium hydroxide (50%, 8 mL) was added slowly under vigorous stirring and the resulting mixture was stirred at ambient temperature for twenty hours. Water was added and the mixture was extracted three times with ether. The combined organic extract was washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography on silica gel using 2% ethyl acetate in heptane as eluent. Concentration of the appropriate fractions afforded 1.40 g (90% yield) of the title compound as an oil. 1H-NMR (300 MHz, CDCl3): δ 0.95 (t, 3H), 1.41 (d, 3H), 1.48 (s, 9H), 1.48-1.66 (m, 4H), 2.05 (m, 4H), 2.83 (m, 8H), 3.35 (m, 1H), 3.55 (m, 1H), 3.79 (q, 1H), 5.32-5.44 (m, 10H).

Aufarbeitung

  1. stirringthe resulting mixture was stirred at ambient temperature for twenty hours
  2. extractionthe mixture was extracted three times with ether
  3. extractionThe combined organic extract
  4. washwas washed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by flash chromatography on silica gel using 2% ethyl acetate in heptane as eluent

Quellen und Nachweise

ORD-Eintrag
ord-07caf6a8b2a14f6481c3773f66f89098
Quelldatensatz
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09394228B2

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