反应详情

In 120 ml of ethanol, 8.0 g of ethyl 2-[5-(4-quinolin-2-ylpiperazin-1-yl)pentanoylamino]cyclohex-1-enecarboxylate as synthesized in above Step 4-1-C was dissolved, and to the solution 60 ml of hydrazine monohydrate was added, followed by 4 hours' heating under reflux. Distilling the solvent off under reduced pressure, the residue was dissolved in chloroform, washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over anhydrous magnesium sulfate. Distilling the solvent off under reduced pressure, the residue was purified on silica gel column chromatography (chloroform:methanol=50:1) to provide 3.8 g (51%) of 3-amino-2-[4-(4-quinolin-2-ylpiperazin-1-yl)butyl]-5,6,7,8-tetrahydro-3H-quinazolin-4-one.

1. dissolutionwas dissolved
2. temperature' heating
3. temperatureunder reflux
4. distillationDistilling the solvent off under reduced pressure
5. dissolutionthe residue was dissolved in chloroform
6. washwashed with saturated aqueous sodium hydrogencarbonate solution and saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationDistilling the solvent off under reduced pressure
9. customthe residue was purified on silica gel column chromatography (chloroform:methanol=50:1)