Reaktion #45195

ord-db50c57ccac04da18f71f240ba724e5e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONmixed at room temperature until clear
  2. 2
    workup.ADDITIONmixed at room temperature until clear (in case of the presence of amorphous silica
  3. 3
    Sonstigeto precipitate the complex
  4. 4
    Sonstigedried immediately at 180° C.

Vorschrift

23.9 g of a 45% potassium hydroxide solution (0.192 moles) was added to 767 g water and mixed at room temperature until clear. 40.0 g alpha-lipoic acid (98%, 0.190 moles) was added to the potassium hydroxide solution and mixed at room temperature until clear (in case of the presence of amorphous silica as flowing agent the solution will be slightly cloudy). 221.7 g alpha cyclodextrin (9.2% water content, 0.207 moles) was added and stirred for 60 minutes at room temperature. 0.192 moles of 37% hydrochloric acid was added to precipitate the complex. With a minimal molar excess of hydrochloric acid in comparison to the potassium hydroxide used the final pH of the solution was about pH 3. The final aqueous mixture is spray dried immediately at 180° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737269B2uspto-grants-2010_06