Scandium(3+);trichloride → HCID 178484171, Verbindung

HRID 1256862

Reaktionsgleichung

Reaktionsgleichung von HRID 1256862
[Cl-].[Sc+3:2].[Cl-].[Cl-].[CH3:5][N:6]([CH:8]([Li])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:7]>O1CCCC1>[CH3:5][N:6]([CH:8]([Sc:2]([CH:8]([N:6]([CH3:7])[CH3:5])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH:8]([N:6]([CH3:7])[CH3:5])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:7]

Komponenten

4

Edukt 2

HCID 10176216Scandium(3+);trichlorideHCID 178506893HCID 178506893, Verbindung

Produkt 1

HCID 178484171HCID 178484171, VerbindungAusbeute 81,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

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%).

Aufarbeitung

  1. customto prepare a suspension liquid, which
  2. additionwas added dropwise
  3. stirringby stirring for 12 hours
  4. customwas removed
  5. extractionthe target compound was extracted with toluene
  6. custompurified by recrystallization

Quellen und Nachweise

ORD-Eintrag
ord-70f3059757874f3492a0025b58210e23
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08461270B2

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