反应详情

A solution of 0.75 g (4.02 mMol) of methyl 5-amino-6-chloro-nicotinate and 0.43 g=0.35 ml (4.5 mMol) of methoxyacetylchloride in 20 ml of chlorobenzene was stirred for one hour at 110° C. After the solvent had been removed in vacuo the crude product obtained was purified by flash chromatography (silica gel; methylene chloride/ethanol=100:1), evaporated down again in vacuo and then digested with petroleum ether. Yield: 0.55 g (53% of theory) light yellow amorphous solid, Rf value: 0.33 (silica gel; ethyl acetate/petroleum ether=1:4)

1. customAfter the solvent had been removed in vacuo the crude product
2. customobtained
3. customwas purified by flash chromatography (silica gel; methylene chloride/ethanol=100:1)
4. customevaporated down again in vacuo