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Sodium Hydroxide → 7-(2,4,6-Triiodophenoxy)heptanoic acid

HRID 2222721
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2222721
[I:1][C:2]1[CH:19]=[C:18]([I:20])[CH:17]=[C:16]([I:21])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13]CC)=[O:12].[OH-].[Na+]>C(O)C>[I:1][C:2]1[CH:19]=[C:18]([I:20])[CH:17]=[C:16]([I:21])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 22939821Ethyl 7-(2,4,6-triiodophenoxy)heptanoate

Produkt 1

HCID 229398227-(2,4,6-Triiodophenoxy)heptanoic acidAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Ethanol (95%, 30 mL) was added with of ethyl 7-(2,4,6-triiodophenoxy)-heptanoate (4.0 g) and the mixture was refluxed for dissolution, and the solution was added with sodium hydroxide (0.5 g) and further refluxed for 1.5 hours. The crystals obtained were separated by filtration, washed with ethanol and added with dichloromethane and 1 N hydrochloric acid to conduct extraction twice with dichloromethane. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was removed. The resulting residue was purified by silica gel column chromatography to obtain 7-(2,4,6-triiodophenoxy)heptanoic acid (3.4 g, yield: 90%).

Aufarbeitung

  1. temperaturethe mixture was refluxed for dissolution
  2. temperaturefurther refluxed for 1.5 hours
  3. customThe crystals obtained
  4. customwere separated by filtration
  5. washwashed with ethanol
  6. additionadded with dichloromethane and 1 N hydrochloric acid
  7. extractionextraction twice with dichloromethane
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. customthe solvent was removed
  10. customThe resulting residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-6f2af0f308884e1e90824cfa8181237b
Quelldatensatz
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07371877B2

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