Reaktion #358194

Reaktionsgleichung

3-tert-butyl-6,6-dimethylfulvene

2,7-di-tert-butylfluorene

hexane

n-butyllithium

→

powdery white solid

Ausbeute 71.5%

2-(3-tert-butyl-5-methylcyclopentadienyl)-2-(2,7-di-tert-butylfluorenyl)propane

Ausbeute 71.5%

Lösungsmittel

water

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGby stirring at room temperature overnight
2. 2
   Sonstigereaction
3. 3
   workup.ADDITIONwas added
4. 4
   ExtraktionThe organic phase was extracted with ether
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONFrom the resulting solution, the solvent was distilled off
7. 7
   Sonstigeto obtain a crude yellow solid
8. 8
   WaschenThe solid was washed with methanol

Vorschrift

To a solution of 2.45 g (8.80 mmol) of 2,7-di-tert-butylfluorene in 50 ml of THF, 5.67 ml (9.24 mmol) of a hexane solution of n-butyllithium was dropwise added in a nitrogen atmosphere at 0° C., followed by stirring at room temperature overnight. To the resulting solution, a solution of 2.85 g (17.6 mmol) of 3-tert-butyl-6,6-dimethylfulvene in 30 ml of THF was successively dropwise added in a nitrogen atmosphere at 0° C., followed by stirring at room temperature overnight to perform reaction. After the reaction, 30 ml of water was added. The organic phase was extracted with ether and dried over anhydrous magnesium sulfate. From the resulting solution, the solvent was distilled off to obtain a crude yellow solid. The solid was washed with methanol to obtain 2.77 g of a powdery white solid (yield: 71.5%.The analyzed values are given below.

Quelle