反应详情

Monomethyl glutarate (3.32 g) is dissolved in chloroform (50 ml) and thereto are added thionyl chloride (1.75 ml) and N,N-dimethylformamide (one drop). After stirring for 1.5 hours at the same temperature, the reaction solution is cooled, and thereto are added 3-amino-N-(5-chloropyridin-2-yl)benzofuran-2-carboxamide (5.00 g) obtained in Reference Example 80 and pyridine (7.0 ml). After stirring for 2.5 hours at room temperature, the reaction solution is poured into 5% hydrochloric acid and extracted with chloroform. The organic layer is washed successively with saturated brine, a saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over sodium sulfate, and evaporated to remove the solvent under reduced pressure. The resulting residue is suspended in diisopropyl ether and the precipitates are collected by filtration to give methyl 5-[(2-{[(5-chloropyridin-2-yl)amino]carbonyl}benzofuran-3-yl)amino]-5-oxopentanoate (6.16 g). APCI-MS M/Z:416/418[M+H]+

1. temperaturethe reaction solution is cooled
2. stirringAfter stirring for 2.5 hours at room temperature
3. extractionextracted with chloroform
4. washThe organic layer is washed successively with saturated brine
5. dry with materiala saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over sodium sulfate
6. customevaporated
7. customto remove the solvent under reduced pressure
8. filtrationthe precipitates are collected by filtration