反应详情

22.61 g (55.0 mmol) of 4-bromophenyl tert.-butyldiphenylsilyl ether in 40 ml of benzene and 35 ml (55.0 mmol) of a 1.6-molar n-butyllithium solution in hexane are stirred overnight at room temperature under argon and then slowly added dropwise to 4.50 ml (50.0 mmol) of 2,6-difluoropyridine in 40 ml of tetrahydrofuran at 0° C. under argon. After a reaction time of 3 hours at 0° C., sodium chloride solution is added, the resulting mixture is taken up in ether, the organic phase is washed with sodium chloride solution, dried over sodium sulfate, filtered, freed from solvent, and the residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate), giving 6.80 g of 6-(4-tert.-butyldiphenylsilyloxyphenyl)-2-fluoropyridine. ##STR44##

1. washthe organic phase is washed with sodium chloride solution
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. customthe residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate)