反应详情

To a solution of 3.15 g (7.22 mmol) of 5-[N-tert-butoxycarbonyl-N-[3-(trifluoromethanesulfonamido)propan-1-yl]aminomethyl]imidazo[1,2-a]pyridine and 2.65 g (21.65 mmol) of 4-dimethylaminopyridine in 30 ml of chloroform was added dropwise, while stirring at room temperature for 3 minutes, 2.4 ml (21.65 mmol) of trichloroacetyl chloride. The reaction mixture was heated for 15 hours under reflux. After completion of the reaction, the reaction mixture was poured into ice-water, which was neutralized with a saturated aqueous solution of sodium hydrogencarbonate. The solution was extracted with 150 ml of chloroform. The organic layer was washed with 250 ml of a saturated aqueous saline solution and dried over magnesium sulfate. The solvent was then distilled off under reduced pressure. The residue was purified by silicagel column chromatography (eluent: chloroform/methanol=100:1) to give 2.31 g of the desired compound (54.8%, pale yellow liquid).

1. temperatureThe reaction mixture was heated for 15 hours
2. temperatureunder reflux
3. customAfter completion of the reaction
4. extractionThe solution was extracted with 150 ml of chloroform
5. washThe organic layer was washed with 250 ml of a saturated aqueous saline solution
6. dry with materialdried over magnesium sulfate
7. distillationThe solvent was then distilled off under reduced pressure
8. customThe residue was purified by silicagel column chromatography (eluent: chloroform/methanol=100:1)