Reaktion #41714

ord-37b33ba6a8ca458180a3763efdda179d

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction liquid

Vorschrift

The reaction liquid was found by gas chromatography (GC) analysis to contain 59.0% of the target compound, 3,3′-bis(1-hydroxy-1-trifluoromethyl-2,2,2-trifluoroethyl)-4,4′-oxydianiline, 9.3% of 3-(1-hydroxy-1-trifluoromethyl-2,2,2-trifluoroethyl)-4,4′-oxydianiline, and 28.8% of the total of various imines produced by the reaction of hexafluoroacetone with the amine moiety of 4,4′-oxydianiline. 50 ml of toluene were added to the reaction liquid, followed by heating dissolution. After cooling, the precipitated solid matter was filtered, followed by vacuum drying. 15.2 g of crude 3,3′-bis(1-hydroxy-1-trifluoromethyl-2,2,2-trifluoroethyl)-4,4′-oxydianiline (yield: 91%; purity: 88.2%) were obtained. This crude product was recrystallized in toluene, thereby obtaining 12.0 g of the target 3,3′-bis(1-hydroxy-1-trifluoromethyl-2,2,2-trifluoroethyl)-4,4′-oxydianiline (yield: 72%; purity: 94.5%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728103B2uspto-grants-2010_06