Hydrochloric Acid → HCID 86620292、化合物
反応式
[O:1]1CCO[CH:2]1[C:6]1[C:7]([F:22])=[C:8]([N:13]([CH2:20][CH3:21])[CH2:14][C:15]2[NH:16][CH:17]=[N:18][CH:19]=2)[CH:9]=[CH:10][C:11]=1[F:12].Cl>O1CCCC1>[CH2:20]([N:13]([CH2:14][C:15]1[NH:16][CH:17]=[N:18][CH:19]=1)[C:8]1[C:7]([F:22])=[C:6]([C:11]([F:12])=[CH:10][CH:9]=1)[CH:2]=[O:1])[CH3:21]参加物
4
実験手順
To a stirred solution of (3-[1,3]dioxolan-2-yl-2,4-difluoro-phenyl)-ethyl-(3H-imidazol-4-ylmethyl)-amine (0.22 g, 0.70 mmol) in tetrahydrofuran (5 ml) was added a 3 N aqueous solution of hydrochloric acid (0.93 ml, 2.79 mmol) and the mixture was stirred at room temperature for 48 h. The mixture was then concentrated in vacuo and the residue taken up in ethyl acetate and washed with 1 N aq. sodium hydroxide solution. The layers were separated and the aqueous phase was back extracted twice with ethyl acetate. The combined organic phases were washed with saturated brine, then dried over magensium sulfate and concentrated in vacuo. The residue was purified by flash chromatography (column: Isolute® Flash-NH2 (Separtis); eluent: methanol/dichloromethane gradient) to yield a yellow gum (111 mg, 48%); MS (ISP): 266.0 ((M+H)+.).