反应详情

In 10 ml of anhydrous acetonitrile was suspended 1.05 g of ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-hydroxynicotinoyl]acetate, and 450 mg of triethylamine and 1.22 g of diphenylphosphoryl azide were added thereto with ice-cooling, after which the resulting mixture was subjected to reaction at room temperature for 4 hours. To this reaction mixture were added 50 ml of ethyl acetate and 50 ml of water, and the organic layer was separated, and then dried over anhydrous magnesium sulfate. The solvent was removed by ditillation under reduced pressure, and the residue thus obtained was purified by a column chromoatography [Wako Silica Gel C-200, eluant: benzene] to obtain 550 mg (yield 48.9%) of ethyl 2-[6-azido-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetate having a melting point of 130°-131° C.

1. additionwere added
2. temperaturewith ice-cooling
3. customafter which the resulting mixture was subjected to reaction at room temperature for 4 hours
4. customthe organic layer was separated
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was removed by ditillation under reduced pressure
7. customthe residue thus obtained
8. customwas purified by a column chromoatography [Wako Silica Gel C-200, eluant: benzene]