2,6-Di-tert-butylphenol → HCID 66586998, Verbindung

Temperatur

100 °C

A flask with a stirring bar was charged with a mixture of compound 1 (1.000 g, 1.54 mmol), PdCl2(PPh3)2 (0.0588 g, 0.065 mmol), a few crystals of 2,6-ditert-butylphenol, and toluene (15.0 mL). The mixture was heated to 100° C. under nitrogen, and tributylvinyltin (1.125 g, 3.534 mmol) was added dropwise. The mixture was further heated for 23 hours. It was subsequently diluted with 60 mL of ether and treated with KF solution (˜10%). The mixture was stirred for 20 hours and followed by filtration to remove the insoluble solid. The organic layer was washed with water and dried over anhydrous MgSO4. After removal of the solvent, the residue was purified by column chromatography with n-hexane as eluent to afford 0.650 g of compound 2.

1. temperatureThe mixture was further heated for 23 hours
2. filtrationfollowed by filtration
3. customto remove the insoluble solid
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous MgSO4
6. customAfter removal of the solvent
7. customthe residue was purified by column chromatography with n-hexane as eluent

ORD-Eintrag

ord-4bbe3177a8784ef1a311010b986c19fd

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08969509B2