Reaktion #319029

ord-67bcd222491a4222b5b86b412c77e62b

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added to the solution
  2. 2
    Sonstigewere precipitated
  3. 3
    FiltrationThe precipitated crystals were recovered by filtration
  4. 4
    Sonstigerecrystallized from ethanol

Vorschrift

In 50 ml of dioxane was dissolved 1.3 g of dimethyl 2',3'-methylenedioxy-2,3,4,4'-tetramethoxy-1,1'-biphenyl-6,6'-dicarboxylate obtained in Example 2, and 10 mg of 5% potassium hydroxide was added to the solution. The mixture was heated at 70° C. and stirred overnight. When the pH value of the mixture was adjusted to 1 by 3N hydrochloric acid, crystals were precipitated. The precipitated crystals were recovered by filtration and recrystallized from ethanol to obtain 1.12 g of 2',3'-methylenedioxy-2,3,4,4'-tetramethoxy-1,1'-biphenyl-6,6'-dicarboxylic acid having the following physical properties (the yield was 92%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04849448uspto-grants-1989_07