반응 #939018

ord-f8e59d31c55344dab18d4c459cf6a61a

반응 방정식

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

반응 조건

온도
115°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to react
  2. 2
    workup.ADDITIONwas added to the reaction solution
  3. 3
    추출The oily layer was extracted with ether
  4. 4
    세척washed with aqueous sodium hydrogencarbonate
  5. 5
    세척washed with water
  6. 6
    기타dried
  7. 7
    기타The residue was evaporated
  8. 8
    기타to remove the solvent
  9. 9
    workup.DISTILLATIONdistilled

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07252849B2uspto-grants-2007_08