反应详情

1-(4-Piperidinyl)-3,4-dihydrocarbostyril (500 mg), triethylamine (1.2 ml) and pyrrole-2-carboxylic acid (314 mg) are dissolved in dichloromethane (10 ml) and thereto is added dropwise diethyl cyanophosphate (0.82 ml) under ice cooling. The mixture is stirred with ice cooling for 1 hour and then stirred at room temperature for 2 hours. The mixture is poured into water, extracted with chloroform, dried with sodium carbonate and purified by silica gel column chromatography (solvent; dichloromethane:methanol=20:1). The resultant is recrystallized from n-hexane/diethyl ether to give 1-[1-(2-pyrrolylcarbonyl)-4-piperidinyl]-3,4-dihydrocarbostyril (0.2 g), as white powder, m.p. 161°-162° C. (decomposed).

1. stirringstirred at room temperature for 2 hours
2. extractionextracted with chloroform
3. dry with materialdried with sodium carbonate
4. custompurified by silica gel column chromatography (solvent; dichloromethane:methanol=20:1)
5. customThe resultant is recrystallized from n-hexane/diethyl ether