Trifluoroacetic acid → HCID 18447431、化合物

反応式

FC(F)(F)C(O)=O.[CH2:8]([N:15]1[CH:20]2[CH2:21][CH2:22][CH:16]1[CH2:17][CH:18]([NH:23][C:24]1[C:25]([CH3:39])=[C:26]3[C:30](=[CH:31][CH:32]=1)[N:29](C1CCCCO1)[N:28]=[CH:27]3)[CH2:19]2)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(=O)([O-])O.[Na+]>ClCCl>[CH2:8]([N:15]1[CH:20]2[CH2:21][CH2:22][CH:16]1[CH2:17][CH:18]([NH:23][C:24]1[C:25]([CH3:39])=[C:26]3[C:30](=[CH:31][CH:32]=1)[NH:29][N:28]=[CH:27]3)[CH2:19]2)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

実験手順

Trifluoroacetic acid (1 ml) was added to a solution of the N-(8-benzyl-8-azabicyclo[3.2.1]oct-3-yl)-4-methyl-1-tetrahydro-2H-pyran-2-yl-1H-indazol-5-amine (273 mg, 0.634 mmol) obtained in Example 499 in dichloromethane (9 ml), and the resulting mixture was stirred at room temperature for 30 minutes. Then, trifluoroacetic acid (1 ml) was added thereto and stirred for another 30 minutes, and the resulting mixture was poured into a saturated aqueous sodium hydrogencarbonate solution and extracted with chloroform. The extract solution was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by a preparative thin-layer chromatography (200×200×0.5 mm, 6 plates, eluent: chloroform/methanol=6/1) to obtain N-(8-benzyl-8-azabicyclo[3.2.1]oct-3-yl)-4-methyl-1H-indazol-5-amine (142 mg, 65%).