Reaktion #70114

ord-43f62bcafd254a00bdc53b94ba711a8f

Lösungsmittel

Reaktionsbedingungen

Temperatur
81.5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe resulting solution was heated to a reflux temperature
  2. 2
    TemperaturDuring this stirring, every one hour from the start to 1 to 5 hours after the start of refluxing
  3. 3
    workup.WAITas well as after 9 hours
  4. 4
    TemperaturAfter cooling to room temperature
  5. 5
    Sonstigethe reaction liquid
  6. 6
    Einengenwas concentrated under reduced pressure

Vorschrift

In the stream of an argon gas, 80 g of 4-cyclohexene-1,2-dicarboxylic di(2-ethylhexyl)ester (manufactured by Tokyo Chemical Industry Co., Ltd.) and 900 mL of isopropyl alcohol was placed. 660 mL of an aqueous solution of 42.3 g of sodium hydrogen sulfite (manufactured by Wako Pure Chemical Industries, Ltd.) was added. The resulting solution was heated to a reflux temperature, and stirred at 80 to 83° C. for 16 hours. During this stirring, every one hour from the start to 1 to 5 hours after the start of refluxing, as well as after 9 hours and 10 hours, 1.66 g of 2,2′-azobis(isobutyronitrile) (manufactured by Wako Pure Chemical Ltd.) was added. After cooling to room temperature, the reaction liquid was concentrated under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08535812B2uspto-grants-2013_09