Reaktion #939018

ord-f8e59d31c55344dab18d4c459cf6a61a

Reaktionsgleichung

O=S(=O)(O)O
sulfuric acid
CCCCI
butyl iodide
II
iodine
CCOC(=O)CCCCC(=O)O.[Cl-]
adipic acid monoethyl ester chloride
CCCCC(=O)CCCCC(=O)OCC
Ethyl 6-Oxodecanoate

Reaktionsbedingungen

Temperatur
115°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto react
  2. 2
    workup.ADDITIONwas added to the reaction solution
  3. 3
    ExtraktionThe oily layer was extracted with ether
  4. 4
    Waschenwashed with aqueous sodium hydrogencarbonate
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigedried
  7. 7
    SonstigeThe residue was evaporated
  8. 8
    Sonstigeto remove the solvent
  9. 9
    workup.DISTILLATIONdistilled

Vorschrift

A mixture of activated zinc-copper catalyst (11.5 g), butyl acetate (4 g), toluene (5 g), butyl iodide (15 g) and iodine (3 mg) was heated at 110-120° C. for 2 hours. The mixture was then added dropwise with adipic acid monoethyl ester chloride(15.7 g) at 0° C., and then was allowed to react. After the reaction was completed, ice-cooled water was added to the reaction solution, and then decomposed with dilute sulfuric acid. The oily layer was extracted with ether, washed with aqueous sodium hydrogencarbonate, washed with water, and then dried. The residue was evaporated to remove the solvent, and then distilled, thereby giving ethyl 6-oxodecanoate (8.1 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07252849B2uspto-grants-2007_08