1-(3-Aminopropyl)-4-methylpiperazine → HCID 68857366, 화합물

반응식

C(N(C(C)C)CC)(C)C.[NH2:10][CH2:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]1.[CH:21]1([NH:24][C:25]([C:27]2[C:35]3[CH:34]=[C:33]([C:36]4[C:41]([Cl:42])=[CH:40][N:39]=[C:38](Cl)[N:37]=4)[S:32][C:31]=3[C:30]([O:44][CH3:45])=[CH:29][CH:28]=2)=[O:26])[CH2:23][CH2:22]1>O1CCOCC1>[CH:21]1([NH:24][C:25]([C:27]2[C:35]3[CH:34]=[C:33]([C:36]4[C:41]([Cl:42])=[CH:40][N:39]=[C:38]([NH:10][CH2:11][CH2:12][CH2:13][N:14]5[CH2:15][CH2:16][N:17]([CH3:20])[CH2:18][CH2:19]5)[N:37]=4)[S:32][C:31]=3[C:30]([O:44][CH3:45])=[CH:29][CH:28]=2)=[O:26])[CH2:22][CH2:23]1

참가 물질

실험 절차

Diisopropylethylamine (1.10 mL, 5.78 mmol) and 1-(3-aminopropyl)-4-methylpiperazine (545 mg, 3.47 mmol) are added to a stirred suspension of 2-(2,5-dichloropyrimidin-4-yl)-7-methoxybenzo[b]thiophene-4-carboxylic acid cyclopropylamide (1.14 g, 2.89 mmol) in dry 1,4-dioxane (25 mL) at room temperature. The resultant mixture is heated in an oil bath at 97° C. for 2 days. At room temperature the mixture is filtered off and the solid is washed with MeOH to give the title compound as a solid (600 mg, 33% yield). The filtrate is concentrated and the residue is purified by HLB cartridge eluting with NH4HCO3 (pH=8) in CH3CN 1:0 to 0:1, and then by Stratta® column, eluting with dichloromethane in MeOH 12:1 to 4:1, to give an additional 339 mg of the title compound as a yellow solid. ES+(m/z) 515 (35Cl) and 517 (37Cl) [M+H].