反应详情

A mixed solution of 17 ml of bromine, 90 g of potassium bromide and 450 ml of water was added dropwise into a mixture of 60 g of 2-benzyl-6-methoxypyridine (Production Example 2-b), 90 g of potassium bromide, 450 ml of water, 20 g of potassium hydroxide and 2.5 g of tetraammonium chloride over 2 hours under stirring in an ice bath. After stirring overnight as it was, sodium sulfite was added thereto and the mixture was extracted with hexane. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography to elute with 0.5-1.5% of ethyl acetate/hexane, to give 72.5 g of the target compound.

1. stirringAfter stirring overnight as it
2. extractionthe mixture was extracted with hexane
3. washThe organic phase was washed with water and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was removed
6. washto elute with 0.5-1.5% of ethyl acetate/hexane