反应 #939018

ord-f8e59d31c55344dab18d4c459cf6a61a

反应方程式

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

反应条件

温度
115°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to react
  2. 2
    workup.ADDITIONwas added to the reaction solution
  3. 3
    萃取The oily layer was extracted with ether
  4. 4
    洗涤washed with aqueous sodium hydrogencarbonate
  5. 5
    洗涤washed with water
  6. 6
    其他dried
  7. 7
    其他The residue was evaporated
  8. 8
    其他to remove the solvent
  9. 9
    workup.DISTILLATIONdistilled

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07252849B2uspto-grants-2007_08