Toluene → HCID 12899429、化合物

反応式

[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:16])[NH:11]2.[CH:17]1[CH:18]=[CH:19][C:20]([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)=[CH:21][CH:22]=1.C1(C)C=CC=CC=1.CCCCCC>C(Cl)(Cl)Cl>[ClH:1].[C:20]1([N:23]2[CH2:28][CH2:27][N:26]([CH2:2][CH2:3][CH2:4][O:5][C:6]3[CH:15]=[CH:14][CH:13]=[C:12]4[C:7]=3[CH2:8][CH2:9][C:10](=[O:16])[NH:11]4)[CH2:25][CH2:24]2)[CH:21]=[CH:22][CH:17]=[CH:18][CH:19]=1

参加物

実験手順

4.8 grams of 5-(3-chloropropoxy)-3,4-dihydrocarbostyril and 4 g of phenylpiperazine are mixed with 40 ml of toluene and heated for 24 hours under refluxing conditions. Then the reaction mixture is concentrated under reduced pressure to dryness. The residue thus obtained is dissolved in 80 ml of chloroform and the chloroform layer is washed twice with 5.0% of sodium hydrogencarbonate aqueous solution, further washed twice with water, dried with anhydrous sodium sulfate and chloroform is removed by distillation. To the residue thus obtained is added hexane and the insoluble material is collected by filtration, then the insoluble material is dissolved in 30 ml of 5% HCl-methanol solution and concentrated under reduced pressure to dryness. Then the residue thus obtained is recrystallized from methanol-ether to obtain 3.2 of 5-[3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril monohydrochloride in the form of colorless crystals with a melting point of 262° C. (decomposition).