反应详情

温度

100 °C

To a solution of 785 mg (2.00 mmol) of 2-ethyl-5-[N-[5-(trifluoromethanesulfonamido)pentan-1-yl]aminomethyl]imidazo[1,2-a]pyridine in 5 ml of acetic acid was added 2.25 ml (30.00 mmol) of a 37% aqueous solution of formalin. The mixture was heated for 30 minutes at 100° C. The solvent was then distilled off under reduced pressure. The residue was dissolved in 100 ml of a saturated aqueous solution of potassium carbonate. This solution was neutralized, under ice-cooling, with 1N HCl, which was extracted twice with 100 ml of chloroform. The organic layer was dried over magnesium sulfate, then the solvent was distilled off under reduced pressure. The residue was purified by silicagel column chromatography (eluent: chloroform/methanol=20:1) to give 527 mg of the desired compound (65.2%, colorless liquid).

1. distillationThe solvent was then distilled off under reduced pressure
2. dissolutionThe residue was dissolved in 100 ml of a saturated aqueous solution of potassium carbonate
3. temperaturecooling, with 1N HCl, which
4. extractionwas extracted twice with 100 ml of chloroform
5. dry with materialThe organic layer was dried over magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe residue was purified by silicagel column chromatography (eluent: chloroform/methanol=20:1)