反应详情

A mixture of 1-isopropyl-4-oxo-4,5-dihydroimidazo[1,5-a]-quinoxaline-7-carboxyic acid as synthesized in above Example 8, 271 mg, dimethylamine hydrochloride 90 mg, 1-hydroxybenzotriazole 230 mg, 4-dimethylaminopyridine 24 mg, pyridine 6.8 mL and 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride 288 mg was stirred for 18.5 hours in nitrogen atmosphere. After distilling the solvent off, 25 mL of water was added to the residue and heated under reflux. Cooling the reaction liquid off, the precipitated crystals were recovered by filtration and washed successively with water, hexane and then with diethyl ether. Drying the crystals by heating under reduced pressure, 235 mg of the title compound was obtained.

1. distillationAfter distilling the solvent off, 25 mL of water
2. additionwas added to the residue
3. temperatureheated
4. temperatureunder reflux
5. temperatureCooling
6. customthe reaction liquid off, the precipitated crystals
7. filtrationwere recovered by filtration
8. washwashed successively with water, hexane
9. customDrying the crystals
10. temperatureby heating under reduced pressure