反应详情

To a solution of 7.69 g (18.56 mmol) of 5-[N-tert-butoxycarbonyl-N-(4-trifluoroacetamidobutan-1-yl)amino methyl]imidazo[1,2-a]pyridine and 10.20 g (83.52 mmol) of 4-(N,N-dimethylamino)pyridine in 100 ml of THF was added 6.21 ml (55.67 mmol) of trichloroacetyl chloride. The reaction mixture was heated for 16 hours under reflux. The reaction mixture was poured into ice-water, and extracted with 100 ml of ethyl acetate. The organic layer was washed with 150 ml of a saturated aqueous saline solution, dried over magnesium sulfate, and distilled off the solvent under reduced pressure. The residue was purified by silica gel column chromatography (eluent; chloroform) to afford 4.98 g of the desired compound (48.0%, a pale yellow amorphous).

1. temperatureThe reaction mixture was heated for 16 hours
2. temperatureunder reflux
3. extractionextracted with 100 ml of ethyl acetate
4. washThe organic layer was washed with 150 ml of a saturated aqueous saline solution
5. dry with materialdried over magnesium sulfate
6. distillationdistilled off the solvent under reduced pressure
7. customThe residue was purified by silica gel column chromatography (eluent; chloroform)