反应详情

Into 100 ml of ethanol were added 2.7 g of 6-(3-ethoxycarbonylpropoxy)carbostyril, 0.5 g of sodium ethylate and 5 ml of N-(2-hydroxyethyl)cyclohexylamine and reacted in an autoclave under a pressure of 110 atomospher at 140°-150° C. for 6 hours. After the reaction was completed, the reaction mixture was cooled and was concentrated under a reduced pressure. The residue thus obtained was dissolved in 200 ml of chloroform and washed with 1% K2CO3 aqueous solution, a diluted hydrochloric acid and water in this order, then dried with anhydrous sodium sulfate. Then the solvent was removed by distillation and the residue thus obtained was purified by a silica-gel column chromatography [the silica-gel used as Wako C-200, and the solvent used was a mixture of chloroform:methanol=20:1 (V/V)]. The crude crystals thus obtained was recrystallized from chloroform-petroleum ether to obtain 0.9 g of 6-{3-[N-(2-hydroxyethyl)-N-cyclohexylaminocarbonyl]propoxy}carbostyril as in the form colorless needle-like crystals. Melting point: 165°-166° C.

1. temperaturethe reaction mixture was cooled
2. concentrationwas concentrated under a reduced pressure
3. customThe residue thus obtained
4. washwashed with 1% K2CO3 aqueous solution
5. dry with materiala diluted hydrochloric acid and water in this order, then dried with anhydrous sodium sulfate
6. customThen the solvent was removed by distillation
7. customthe residue thus obtained
8. customwas purified by a silica-gel column chromatography [the silica-gel
9. additiona mixture of chloroform
10. customThe crude crystals thus obtained
11. customwas recrystallized from chloroform-petroleum ether