[CH3:1][N:2]1[C:6]2=[N:7][C:8]([O:11][CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=3)=[CH:9][CH:10]=[C:5]2[C:4]([N:19]2[CH2:24][CH2:23][N:22](C(OC(C)(C)C)=O)[CH2:21][C:20]2=[O:32])=[CH:3]1.[ClH:33]>C(Cl)Cl.CCOC(C)=O>[ClH:33].[CH3:1][N:2]1[C:6]2=[N:7][C:8]([O:11][CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=3)=[CH:9][CH:10]=[C:5]2[C:4]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][C:20]2=[O:32])=[CH:3]1To a solution of tert-butyl 4-[1-methyl-6-(pyridin-2-ylmethoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]-3-oxopiperazine-1-carboxylate (0.278 g, 0.653 mmol) in DCM (10 mL) is added a saturated solution of hydrogen chloride in EtOAc (6 mL) at room temperature, and the reaction mixture stirred at room temperature for 67 h. The solvent is carefully decanted off and the residue triturated with Et2O/MeOH. The solvent is again decanted off and the residue further triturated with Et2O/MeOH. The resultant residue is dried in vacuo for 3 h. to give the title compound (0.217 g, 0.580 mmol) as a pale yellow solid. MS (m/z): 338 (M+1).
読み込み中…