Reaktion #93445

Reaktionsgleichung

mesityl oxide

2,6 di-tert-butyl-4-mercaptophenol

triethylamine

→

4-Methyl-4-(3,5-di-tert-butyl-4-hydroxyphenylthio)-2-pentanone

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is heated at 50°-55° C. for six hours
2. 2
   Sonstigeretained at 60°-65° C.
3. 3
   Sonstigepurified by flash chromatography
4. 4
   SonstigeThe product is isolated from solution
5. 5
   workup.DISTILLATIONby distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours

Vorschrift

8.48 Grams of mesityl oxide (0.084 moles) is added dropwise to a solution of 21.0 grams of 2,6 di-tert-butyl-4-mercaptophenol (0.088 moles) and one gram of triethylamine in 30 ml of toluene. The mixture is heated at 50°-55° C. for six hours. The solvent is then stripped off under vacuum and the residue retained at 60°-65° C. and 0.20 mm. Hg. for two hours. The residue is dissolved in toluene and purified by flash chromatography using silica gel. The product is isolated from solution by distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours.

Quelle