Reaktion #1344044

ord-70f3059757874f3492a0025b58210e23

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto prepare a suspension liquid, which
  2. 2
    workup.ADDITIONwas added dropwise
  3. 3
    workup.STIRRINGby stirring for 12 hours
  4. 4
    Sonstigewas removed
  5. 5
    Extraktionthe target compound was extracted with toluene
  6. 6
    Sonstigepurified by recrystallization

Vorschrift

1.0 g (6.6 mmol) of anhydrous scandium chloride and 10 mL of tetrahydrofuran (THF) were placed in a 100 mL glass vessel to prepare a suspension liquid, which was stirred at room temperature for 1 hour. 2.8 g (20 mmol) of the above-obtained dimethylaminobenzyllithium dissolved in 20 mL of THF was added dropwise thereto, followed by stirring for 12 hours. After completing the reaction, THF was removed, and the target compound was extracted with toluene and then purified by recrystallization to provide 2.4 g of tris(dimethylaminobenzyl)scandium (Sc (CH2C6H4N(CH3)2-o)3) as pale yellow crystals (yield: 80%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08461270B2uspto-grants-2013_06