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Ethanol → Ethyl 3-iodo-4-methylbenzoate

HRID 13752
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 13752
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>>[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([O:7][CH2:17][CH3:18])=[O:6]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 6216403-Iodo-4-methylbenzoic acid

Produkt 1

HCID 23073518Ethyl 3-iodo-4-methylbenzoate

Versuchsvorschrift

40.61 g of 3-iodo-4-methylbenzoic acid was suspended in 406 ml of ethanol and 9.1 ml of concentrated sulfuric acid was added, and then the mixture was heated at reflux for 24 hours. After the solvent was distilled off under reduced pressure, the residue was mixed with iced water, made basic with an aqueous saturated sodium hydrogen carbonate solution, followed by extraction with ethyl acetate twice. The extracts were washed in turn with water and saturated saline and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 44.44 g of a crude product as a brown oily product.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 24 hours
  3. distillationAfter the solvent was distilled off under reduced pressure
  4. additionthe residue was mixed with iced water
  5. extractionfollowed by extraction with ethyl acetate twice
  6. washThe extracts were washed in turn with water and saturated saline
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e7d713160acb4b798d7d7c899f2643a7
Quelldatensatz
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07728131B2

Notizen zur Reaktion

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