反应详情

3.8 Grams of 6-[3-(p-nitrophenoxycarbonyl)propoxy]carbostyril was dissolved in 40 ml of dimethylformamide, then 1.6 ml of N-(2-hydroxyethyl)cyclohexylamine was added thereto and the reaction mixture was stirred at 60°-70° C. for 12 hours. After the reaction was completed, the solvent was removed by distillation and the residue thus obtained was purified by a silica-gel column chromatography [Silica-gel used was "Wako C-200" and the solvent used was a mixture of chloroform:methanol=20:1 (vol/vol)]. The crude crystals thus obtained was recrystallized from chloroform-petroleum ether to obtain 1.3 g of 6-{3-[N-(2-hydroxyethyl)-N-cyclohexylaminocarbonyl]propoxy}carbostyril as in the form of colorless needle-like crystals. Melting point: 165°-166° C.

1. customthe solvent was removed by distillation
2. customthe residue thus obtained
3. customwas purified by a silica-gel column chromatography [Silica-gel
4. additiona mixture of chloroform
5. customThe crude crystals thus obtained
6. customwas recrystallized from chloroform-petroleum ether